CN106964178B - Dedicated defoaming agent of a kind of phosphoric acid processing and preparation method thereof - Google Patents
Dedicated defoaming agent of a kind of phosphoric acid processing and preparation method thereof Download PDFInfo
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- CN106964178B CN106964178B CN201710251067.6A CN201710251067A CN106964178B CN 106964178 B CN106964178 B CN 106964178B CN 201710251067 A CN201710251067 A CN 201710251067A CN 106964178 B CN106964178 B CN 106964178B
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 239000002518 antifoaming agent Substances 0.000 title claims abstract description 56
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 238000003672 processing method Methods 0.000 title claims description 7
- 229920000570 polyether Polymers 0.000 claims abstract description 135
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 106
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 83
- 239000004135 Bone phosphate Substances 0.000 claims abstract description 45
- PLFFHJWXOGYWPR-HEDMGYOXSA-N (4r)-4-[(3r,3as,5ar,5br,7as,11as,11br,13ar,13bs)-5a,5b,8,8,11a,13b-hexamethyl-1,2,3,3a,4,5,6,7,7a,9,10,11,11b,12,13,13a-hexadecahydrocyclopenta[a]chrysen-3-yl]pentan-1-ol Chemical compound C([C@]1(C)[C@H]2CC[C@H]34)CCC(C)(C)[C@@H]1CC[C@@]2(C)[C@]4(C)CC[C@@H]1[C@]3(C)CC[C@@H]1[C@@H](CCCO)C PLFFHJWXOGYWPR-HEDMGYOXSA-N 0.000 claims abstract description 44
- 150000002334 glycols Chemical class 0.000 claims abstract description 38
- 239000002994 raw material Substances 0.000 claims abstract description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 60
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 57
- 238000000034 method Methods 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 31
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 26
- 229910052799 carbon Inorganic materials 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 20
- 230000032683 aging Effects 0.000 claims description 20
- 235000006408 oxalic acid Nutrition 0.000 claims description 20
- 238000010792 warming Methods 0.000 claims description 20
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 16
- 238000003825 pressing Methods 0.000 claims description 16
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 15
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 15
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 14
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 10
- 229920000136 polysorbate Polymers 0.000 claims description 9
- 235000012424 soybean oil Nutrition 0.000 claims description 8
- 239000003549 soybean oil Substances 0.000 claims description 8
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 5
- 238000000605 extraction Methods 0.000 abstract description 15
- 239000006260 foam Substances 0.000 abstract description 12
- 230000005764 inhibitory process Effects 0.000 abstract description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract description 2
- 230000003254 anti-foaming effect Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000000087 stabilizing effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 8
- 238000012545 processing Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- QBUKAFSEUHGMMX-MTJSOVHGSA-N (5z)-5-[[3-(1-hydroxyethyl)thiophen-2-yl]methylidene]-10-methoxy-2,2,4-trimethyl-1h-chromeno[3,4-f]quinolin-9-ol Chemical group C1=CC=2NC(C)(C)C=C(C)C=2C2=C1C=1C(OC)=C(O)C=CC=1O\C2=C/C=1SC=CC=1C(C)O QBUKAFSEUHGMMX-MTJSOVHGSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 239000002367 phosphate rock Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- QQGISFDJEJMKIL-JAIQZWGSSA-N (5z)-5-[[3-(hydroxymethyl)thiophen-2-yl]methylidene]-10-methoxy-2,2,4-trimethyl-1h-chromeno[3,4-f]quinolin-9-ol Chemical group C1=CC=2NC(C)(C)C=C(C)C=2C2=C1C=1C(OC)=C(O)C=CC=1O\C2=C/C=1SC=CC=1CO QQGISFDJEJMKIL-JAIQZWGSSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 241001411320 Eriogonum inflatum Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000000963 oxybis(methylene) group Chemical group [H]C([H])(*)OC([H])([H])* 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polyethers (AREA)
Abstract
The invention belongs to chemical fields, dedicated defoaming agent and preparation method thereof is processed more particularly to a kind of phosphoric acid, composition includes the raw material of following parts by weight: 10~30 parts of polyether monol, 30~40 parts of polyether Glycols, 20~30 parts of polyether-tribasic alcohol and 5~10 parts of polyethers tetrahydroxylic alcohol；The molecular weight of the polyether monol is 1000~1500, general formula C4H9O(C3H6O)a(C2H4O)bH；The molecular weight of the dihydric alcohol is 2000~3000, and general formula isThe molecular weight of the polyether-tribasic alcohol is 3000~3600, and general formula isThe molecular weight of the polyethers tetrahydroxylic alcohol is 4000~5000, and general formula is C [CH2O(C3H6O)n(C2H4O)mH]4.Defoaming agent of the invention has the characteristics that antifoaming speed is fast, defoaming capacity is strong, the foam inhibition time is long；The operating condition for stabilizing extraction process, realizes the long period oepration at full load of extraction process, brings significant economic benefit to enterprise.
Description
Technical field
The invention belongs to chemical fields, and in particular to dedicated defoaming agent of a kind of phosphoric acid processing and preparation method thereof.
Background technique
Existing phosphoric acid by wet process extracts production process are as follows: ground, sieved, flotation, it is dense after qualified slurry by conveying
It is pumped into extraction tank, is added after concentrated sulfuric acid extraction reaction and band filter or revolving-leaf type filter filtering is transported to by pump, rinse
After obtain required for phosphoric acid,diluted product, due to rock phosphate in powder entrained with organic matter or remain in floating agent and sulphur in ore pulp
Acid reaction generates great amount of carbon dioxide gas, causes extraction slurry to generate a large amount of viscous foams, leads to extraction tank liquid level virtual height, greatly
It measures stable foam to tie up, block extraction tank overdraught channel, tail gas extraction difficult, tail washes system condition deterioration, extracts work
Sequence operation under positive pressure, extraction is fluorine-containing, sour gas is excessive, reduces the fluorine rate of recovery, pollutes environment, corrodes production scene equipment, even
Cause the extraction process underproduction or parking accident；Carry out larger difficult and economic loss to Wet-process Phosphoric Acid Production device band.
In order to reduce influence of the foam to production, it is often necessary to defoaming agent be added and carry out defoaming treatment.However, existing disappear
Infusion cannot play the role of defoaming substantially in high temperature, strong acid environment, or even also occur being aggravated what foam generated by sulfuric acid oxidation
Situation.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of phosphoric acid to process dedicated defoaming agent, processed to eliminate phosphoric acid
The foam that generates in extraction equipment in journey stablizes extraction equipment production technology.
In order to solve the above-mentioned technical problem, the technical solution of the present invention is as follows:
A kind of dedicated defoaming agent of phosphoric acid processing, composition include the raw material of following parts by weight: polyether monol 10~30
Part, 30~40 parts of polyether Glycols, 20~30 parts of polyether-tribasic alcohol and 5~10 parts of polyethers tetrahydroxylic alcohol；The polyether monol
Molecular weight is 1000~1500, general formula C4H9O(C3H6O)a(C2H4O)bH；The molecular weight of the dihydric alcohol is 2000~3000,
General formula isThe molecular weight of the polyether-tribasic alcohol is 3000~3600, and general formula isThe molecular weight of the polyethers tetrahydroxylic alcohol is 4000~5000, and general formula is C [CH2O(C3H6O)n
(C2H4O)mH]4。
Processed in dedicated defoaming agent in phosphoric acid provided by the invention, it is preferable that the polyether monol the preparation method comprises the following steps:
Butanol, the propylene oxide that parts by weight are 100 parts and the hydrogen-oxygen that parts by weight are 0.5~1 part for being 5~10 parts by parts by weight
Change potassium and reaction kettle is added, stirring is warming up to 120~130 DEG C, is pressurized to 0.85~0.95MPa, reacts 8~12h；Then weight is added
The ethylene oxide that number is 2~30 parts is measured, under conditions of temperature is 90~110 DEG C, pressure is 0.4-0.6MPa, reaction 6~
10h；3~10h of constant temperature aging under conditions of 90~100 DEG C；Temperature be 100~110 DEG C, vacuum degree be -500mmHg~-
It is vacuumized under conditions of 900mmHg, obtains thick polyether monol；Under conditions of 120~140 DEG C, add into thick polyether monol
Enter the oxalic acid that parts by weight are 0.5~1 part to neutralize, adds the active carbon that parts by weight are 1~5 part and decolourize, after decoloration
Through plate and frame filter press filters pressing under conditions of pressure is 0.3MPa, polyether monol is obtained.
Processed in dedicated defoaming agent in phosphoric acid provided by the invention, it is preferable that the polyether Glycols the preparation method comprises the following steps:
It is 0.5~1 by propylene glycol, the propylene oxide that parts by weight are 90~100 parts and parts by weight that parts by weight are 10~15 parts
Reaction kettle is added in the potassium hydroxide of part, and stirring is warming up to 100~130 DEG C, is pressurized to 0.8~0.9MPa, reacts 8~12h；Then
The ethylene oxide that parts by weight are 10~30 parts is added, is 90~120 DEG C in temperature, under conditions of pressure is 0.2-0.5MPa,
React 6~10h；It is 3~10h of constant temperature aging in 120~130 DEG C of conditions；Temperature be 100~110 DEG C, vacuum degree be -500
It is vacuumized under conditions of~-800mmHg, obtains thick polyether Glycols；Under conditions of 110~120 DEG C, into thick polyether Glycols
The oxalic acid that parts by weight are 0.5~1 part is added to neutralize, adds the active carbon that parts by weight are 1~5 part and decolourizes, decolourize
By plate and frame filter press filters pressing under conditions of pressure is 0.2MPa, polyether Glycols are obtained.
Processed in dedicated defoaming agent in phosphoric acid provided by the invention, it is preferable that the polyether-tribasic alcohol the preparation method comprises the following steps:
It is 0.5~1 part by glycerol, the propylene oxide that parts by weight are 80~100 parts and parts by weight that parts by weight are 15~25 parts
Potassium hydroxide reaction kettle is added, stirring is warming up to 110~150 DEG C, is pressurized to 0.8~0.95MPa, reacts 8~12h；Then
The ethylene oxide that parts by weight are 5~40 parts is added, is 110~120 DEG C in temperature, under conditions of pressure is 0.2~0.5MPa,
React 6~10h；It is 3~10h of constant temperature aging in 100~120 DEG C of condition of temperature；It is 100~130 DEG C, vacuum degree in temperature
To vacuumize under conditions of -500~-800mmHg, thick polyether-tribasic alcohol is obtained；Under conditions of 100~130 DEG C, to thick polyethers three
The oxalic acid that parts by weight are 0.5~1 part is added in first alcohol to neutralize, adds the active carbon that parts by weight are 1~5 part and is taken off
Color obtains polyether-tribasic alcohol through plate and frame filter press filters pressing under conditions of pressure is 0.2MPa after decoloration.
Processed in dedicated defoaming agent in phosphoric acid provided by the invention, it is preferable that the polyethers tetrahydroxylic alcohol the preparation method comprises the following steps:
By pentaerythrite, the propylene oxide that parts by weight are 80~120 parts and parts by weight that parts by weight are 10~15 parts be 0.5~
Reaction kettle is added in 1 part of potassium hydroxide, and stirring is warming up to 90~110 DEG C, is pressurized to 0.8~1MPa, reacts 8~12h；Then plus
Enter the ethylene oxide that parts by weight are 0~40 part, under conditions of temperature is 110~130 DEG C, pressure is 0.2~0.3MPa, instead
Answer 6~10h；3~10h of constant temperature aging under conditions of 130~140 DEG C；Temperature be 100~110 DEG C, vacuum degree be -500
It is vacuumized under conditions of~-800mmHg, obtains thick polyethers tetrahydroxylic alcohol；Under conditions of 100~110 DEG C, into thick polyethers tetrahydroxylic alcohol
The oxalic acid that parts by weight are 0.5~1 part is added to neutralize, adds the active carbon that parts by weight are 1~5 part and decolourizes, decolourize
By plate and frame filter press filters pressing under conditions of pressure is 0.3MPa, polyethers tetrahydroxylic alcohol is obtained.
It is processed in dedicated defoaming agent in phosphoric acid provided by the invention, it is preferable that further include parts by weight be 1~5 part big
The tween that the sapn and parts by weight that soya-bean oil, parts by weight are 1~3 part are 0.5~2 part.
It is a further object of the present invention to provide the processing methods that a kind of phosphoric acid processes dedicated defoaming agent, which is characterized in that presses
Parts by weight weigh polyether monol, polyether Glycols, polyether-tribasic alcohol and polyethers tetrahydroxylic alcohol and are added in agitator tank, 70~80
It is stirred evenly under conditions of DEG C and processes dedicated defoaming agent to get the phosphoric acid.
In the processing method that phosphoric acid provided by the invention processes dedicated defoaming agent, it is preferable that weigh in parts by weight poly-
Ether monohydric alcohol, polyether Glycols, polyether-tribasic alcohol, polyethers tetrahydroxylic alcohol, soybean oil, sapn and tween are added in agitator tank, 70
It is stirred evenly under conditions of~80 DEG C and processes dedicated defoaming agent to get the phosphoric acid.
By adopting the above technical scheme, due to the conjunction of polyether monol, polyether Glycols, polyether-tribasic alcohol and polyethers tetrahydroxylic alcohol
Reason proportion, generates synergistic effect, so that defoaming effect and foam-inhibiting effect significantly increase；The addition of soybean oil, sapn and tween into
One step increases the defoaming and foam inhibition effect of the defoaming agent；Defoaming agent of the invention is suitable for playing under high temperature, strong acid environment good
Good defoaming effect can guarantee that gas-guide pipeline is unimpeded, at effective recycling by the highly stable control of froth bed in 0~10cm
Harmful exhaust is managed, realizes fluorine resource recycling, reduces field device corrosion and atmosphere pollution；Stabilize the behaviour of extraction process
Make condition, realizes its long all oepration at full load of extraction process, bring significant economic benefit to enterprise.
Specific embodiment
Specific embodiments of the present invention will be further explained below.It should be noted that for these implementations
The explanation of mode is used to help understand the present invention, but and does not constitute a limitation of the invention.In addition, invention described below
Technical characteristic involved in each embodiment can be combined with each other as long as they do not conflict with each other.
Embodiment 1
A kind of dedicated defoaming agent of phosphoric acid processing is present embodiments provided, 10 parts of polyether monol is weighed in parts by weight, gathers
In 8 parts of 40 parts of ether dihydric alcohol, 30 parts of polyether-tribasic alcohol and polyethers tetrahydroxylic alcohol addition agitator tanks, stirred under conditions of 70 DEG C equal
It is even to process dedicated defoaming agent to get phosphoric acid.
Above-mentioned polyether monol the preparation method comprises the following steps: by parts by weight be 10 parts butanol, the ring that parts by weight are 100 parts
Reaction kettle is added in the potassium hydroxide that Ethylene Oxide and parts by weight are 0.5 part, and stirring is warming up to 130 DEG C, is pressurized to 0.95MPa, instead
Answer 8h；Then the ethylene oxide that parts by weight are 2 parts, under conditions of temperature is 110 DEG C, pressure is 0.4MPa, reaction is added
10h；Constant temperature aging 3h under conditions of 100 DEG C；It vacuumizes, obtains under conditions of temperature is 100 DEG C, vacuum degree is -500mmHg
Thick polyether monol；Under conditions of 140 DEG C, the oxalic acid that parts by weight are 1 part is added into thick polyether monol and neutralizes, then plus
Entering parts by weight is that 5 parts of active carbon decolourizes, through plate and frame filter press filters pressing under conditions of pressure is 0.3MPa after decoloration,
Obtain polyether monol.
Above-mentioned polyether Glycols the preparation method comprises the following steps: by parts by weight be 10 parts propylene glycol, parts by weight be 90 parts
Reaction kettle is added in the potassium hydroxide that propylene oxide and parts by weight are 1 part, and stirring is warming up to 130 DEG C, is pressurized to 0.9MPa, reacts
12h；Then the ethylene oxide that parts by weight are 30 parts, under conditions of temperature is 120 DEG C, pressure is 0.5MPa, reaction is added
6h；It is constant temperature aging 3h in 130 DEG C of conditions；It vacuumizes, obtains under conditions of temperature is 100 DEG C, vacuum degree is -800mmHg
Thick polyether Glycols；Under conditions of 120 DEG C, the oxalic acid that parts by weight are 0.5 part is added into thick polyether Glycols and neutralizes, then
The active carbon that parts by weight are 5 parts is added to decolourize, is pressed under conditions of pressure is 0.2MPa after decoloration through plate and frame filter press
Filter, obtains polyether Glycols.
Above-mentioned polyether-tribasic alcohol the preparation method comprises the following steps: by parts by weight be 25 parts glycerol, the ring that parts by weight are 80 parts
Reaction kettle is added in the potassium hydroxide that Ethylene Oxide and parts by weight are 1 part, and stirring is warming up to 150 DEG C, is pressurized to 0.8MPa, reacts
12h；Then the ethylene oxide that parts by weight are 40 parts is added, is 120 DEG C in temperature, under conditions of pressure is 0.5MPa, reaction
6h；It is constant temperature aging 10h in 100 DEG C of condition of temperature；It is taken out under conditions of temperature is 130 DEG C, vacuum degree is -800mmHg true
Sky obtains thick polyether-tribasic alcohol；Under conditions of 130 DEG C, it is added into thick polyether-tribasic alcohol in the oxalic acid that parts by weight are 0.5 part
With adding parts by weight is that 1 part of active carbon decolourizes, through plate and frame filter press in the condition that pressure is 0.2MPa after decoloration
Lower filters pressing, obtains polyether-tribasic alcohol.
Above-mentioned polyethers tetrahydroxylic alcohol the preparation method comprises the following steps: by parts by weight be 10 parts pentaerythrite, parts by weight be 120 parts
Propylene oxide and parts by weight be 1 part potassium hydroxide be added reaction kettle, stirring be warming up to 90 DEG C, be pressurized to 1MPa, react
8h；Then the ethylene oxide that parts by weight are 40 parts, under conditions of temperature is 130 DEG C, pressure is 0.3MPa, reaction is added
10h；Constant temperature aging 10h under conditions of 130 DEG C；It is vacuumized under conditions of temperature is 110 DEG C, vacuum degree is -500mmHg,
Obtain thick polyethers tetrahydroxylic alcohol；Under conditions of 100 DEG C, the oxalic acid that parts by weight are 1 part is added into thick polyethers tetrahydroxylic alcohol and neutralizes, then
The active carbon that parts by weight are 5 parts is added to decolourize, is pressed under conditions of pressure is 0.3MPa after decoloration through plate and frame filter press
Filter, obtains polyethers tetrahydroxylic alcohol.
Embodiment 2
A kind of dedicated defoaming agent of phosphoric acid processing is present embodiments provided, 30 parts of polyether monol is weighed in parts by weight, gathers
In 5 parts of 30 parts of ether dihydric alcohol, 20 parts of polyether-tribasic alcohol and polyethers tetrahydroxylic alcohol addition agitator tanks, stirred under conditions of 80 DEG C equal
It is even to process dedicated defoaming agent to get phosphoric acid.
Above-mentioned polyether monol the preparation method comprises the following steps: by parts by weight be 5 parts butanol, the ring that parts by weight are 100 parts
Reaction kettle is added in the potassium hydroxide that Ethylene Oxide and parts by weight are 1 part, and stirring is warming up to 120 DEG C, is pressurized to 0.85MPa, reacts
12h；Then the ethylene oxide that parts by weight are 30 parts, under conditions of temperature is 90 DEG C, pressure is 0.6MPa, reaction is added
6h；Constant temperature aging 10h under conditions of 90 DEG C；It vacuumizes, obtains under conditions of temperature is 110 DEG C, vacuum degree is -900mmHg
Thick polyether monol；Under conditions of 120 DEG C, the oxalic acid that parts by weight are 0.5 part is added into thick polyether monol and neutralizes, then
The active carbon that parts by weight are 1 part is added to decolourize, is pressed under conditions of pressure is 0.3MPa after decoloration through plate and frame filter press
Filter, obtains polyether monol.
Above-mentioned polyether Glycols the preparation method comprises the following steps: by parts by weight be 15 parts propylene glycol, parts by weight be 100 parts
Reaction kettle is added in the potassium hydroxide that propylene oxide and parts by weight are 0.5 part, and stirring is warming up to 110 DEG C, is pressurized to 0.8MPa, instead
Answer 8h；Then the ethylene oxide that parts by weight are 10 parts, under conditions of temperature is 90 DEG C, pressure is 0.2MPa, reaction is added
10h；It is constant temperature aging 10h in 120 DEG C of conditions；It is vacuumized under conditions of temperature is 110 DEG C, vacuum degree is -500mmHg,
Obtain thick polyether Glycols；Under conditions of 110 DEG C, the oxalic acid that parts by weight are 1 part is added into thick polyether Glycols and neutralizes, then
The active carbon that parts by weight are 1 part is added to decolourize, is pressed under conditions of pressure is 0.2MPa after decoloration through plate and frame filter press
Filter, obtains polyether Glycols.
Above-mentioned polyether-tribasic alcohol the preparation method comprises the following steps: by parts by weight be 15 parts glycerol, the ring that parts by weight are 100 parts
Reaction kettle is added in the potassium hydroxide that Ethylene Oxide and parts by weight are 0.5 part, and stirring is warming up to 110 DEG C, is pressurized to 0.95MPa, instead
Answer 8h；Then the ethylene oxide that parts by weight are 5 parts is added, is 110 DEG C in temperature, under conditions of pressure is 0.2MPa, reaction
10h；It is constant temperature aging 3h in 120 DEG C of condition of temperature；It is taken out under conditions of temperature is 100 DEG C, vacuum degree is -500mmHg true
Sky obtains thick polyether-tribasic alcohol；Under conditions of 100 DEG C, it is added into thick polyether-tribasic alcohol in the oxalic acid that parts by weight are 1 part
With adding parts by weight is that 5 parts of active carbon decolourizes, through plate and frame filter press in the condition that pressure is 0.2MPa after decoloration
Lower filters pressing, obtains polyether-tribasic alcohol.
Above-mentioned polyethers tetrahydroxylic alcohol the preparation method comprises the following steps: by parts by weight be 15 parts pentaerythrite, parts by weight be 80 parts
Propylene oxide and parts by weight be 0.5 part potassium hydroxide be added reaction kettle, stirring be warming up to 110 DEG C, be pressurized to 0.8MPa,
React 12h；Then the ethylene oxide that parts by weight are 2 parts is added, under conditions of temperature is 110 DEG C, pressure is 0.2MPa, instead
Answer 6h；Constant temperature aging 3h under conditions of 140 DEG C；It is vacuumized under conditions of temperature is 100 DEG C, vacuum degree is -800mmHg,
Obtain thick polyethers tetrahydroxylic alcohol；Under conditions of 110 DEG C, the oxalic acid that parts by weight are 0.5 part is added into thick polyethers tetrahydroxylic alcohol and neutralizes,
It adds the active carbon that parts by weight are 1 part to decolourize, after decoloration through plate and frame filter press under conditions of pressure is 0.3MPa
Filters pressing obtains polyethers tetrahydroxylic alcohol.
Embodiment 3
A kind of dedicated defoaming agent of phosphoric acid processing is present embodiments provided, 20 parts of polyether monol is weighed in parts by weight, gathers
In 10 parts of 35 parts of ether dihydric alcohol, 25 parts of polyether-tribasic alcohol and polyethers tetrahydroxylic alcohol addition agitator tanks, stirred under conditions of 80 DEG C equal
It is even to process dedicated defoaming agent to get phosphoric acid.
Above-mentioned polyether monol the preparation method comprises the following steps: by parts by weight be 8 parts butanol, the ring that parts by weight are 100 parts
Reaction kettle is added in the potassium hydroxide that Ethylene Oxide and parts by weight are 0.8 part, and stirring is warming up to 115 DEG C, is pressurized to 0.90MPa, instead
Answer 10h；Then the ethylene oxide that parts by weight are 15 parts is added, under conditions of temperature is 100 DEG C, pressure is 0.5MPa, instead
Answer 9h；Constant temperature aging 7h under conditions of 100 DEG C；It is vacuumized under conditions of temperature is 105 DEG C, vacuum degree is -850mmHg,
Obtain thick polyether monol；Under conditions of 135 DEG C, the oxalic acid that parts by weight are 0.7 part is added into thick polyether monol and neutralizes,
It adds the active carbon that parts by weight are 3 parts to decolourize, after decoloration through plate and frame filter press under conditions of pressure is 0.3MPa
Filters pressing obtains polyether monol.
Above-mentioned polyether Glycols the preparation method comprises the following steps: by parts by weight be 12 parts propylene glycol, parts by weight be 100 parts
Reaction kettle is added in the potassium hydroxide that propylene oxide and parts by weight are 0.8 part, and stirring is warming up to 120 DEG C, is pressurized to 0.9MPa, instead
Answer 10h；Then the ethylene oxide that parts by weight are 20 parts is added, under conditions of temperature is 110 DEG C, pressure is 0.4MPa, instead
Answer 8h；It is constant temperature aging 8h in 115 DEG C of conditions；It is vacuumized under conditions of temperature is 110 DEG C, vacuum degree is -600mmHg,
Obtain thick polyether Glycols；Under conditions of 115 DEG C, the oxalic acid that parts by weight are 0.7 part is added into thick polyether Glycols and neutralizes,
It adds the active carbon that parts by weight are 2 parts to decolourize, after decoloration through plate and frame filter press under conditions of pressure is 0.2MPa
Filters pressing obtains polyether Glycols.
Above-mentioned polyether-tribasic alcohol the preparation method comprises the following steps: by parts by weight be 20 parts glycerol, the ring that parts by weight are 90 parts
Reaction kettle is added in the potassium hydroxide that Ethylene Oxide and parts by weight are 0.9 part, and stirring is warming up to 130 DEG C, is pressurized to 0.85MPa, instead
Answer 10h；Then the ethylene oxide that parts by weight are 25 parts is added, under conditions of temperature is 117 DEG C, pressure is 0.3MPa, instead
Answer 8h；It is constant temperature aging 6h in 110 DEG C of condition of temperature；It is taken out under conditions of temperature is 120 DEG C, vacuum degree is -800mmHg true
Sky obtains thick polyether-tribasic alcohol；Under conditions of 100 DEG C, it is added into thick polyether-tribasic alcohol in the oxalic acid that parts by weight are 0.8 part
With adding parts by weight is that 4 parts of active carbon decolourizes, through plate and frame filter press in the condition that pressure is 0.2MPa after decoloration
Lower filters pressing, obtains polyether-tribasic alcohol.
Above-mentioned polyethers tetrahydroxylic alcohol the preparation method comprises the following steps: by parts by weight be 12 parts pentaerythrite, parts by weight be 110 parts
Propylene oxide and parts by weight be 0.8 part potassium hydroxide be added reaction kettle, stirring be warming up to 108 DEG C, be pressurized to 1MPa, instead
Answer 10h；Then the ethylene oxide that parts by weight are 30 parts is added, under conditions of temperature is 120 DEG C, pressure is 0.2MPa, instead
Answer 8h；Constant temperature aging 8h under conditions of 135 DEG C；It is vacuumized under conditions of temperature is 105 DEG C, vacuum degree is -600mmHg,
Obtain thick polyethers tetrahydroxylic alcohol；Under conditions of 105 DEG C, the oxalic acid that parts by weight are 0.7 part is added into thick polyethers tetrahydroxylic alcohol and neutralizes,
It adds the active carbon that parts by weight are 3 parts to decolourize, after decoloration through plate and frame filter press under conditions of pressure is 0.3MPa
Filters pressing obtains polyethers tetrahydroxylic alcohol.
Embodiment 4
A kind of dedicated defoaming agent of phosphoric acid processing is present embodiments provided, 10 parts of polyether monol is weighed in parts by weight, gathers
2 parts of 40 parts of ether dihydric alcohol, 30 parts of polyether-tribasic alcohol, 8 parts of polyethers tetrahydroxylic alcohol, 5 parts of soybean oil, 1 part of sapn and tween addition stirrings
In tank, is stirred evenly under conditions of 70 DEG C and process dedicated defoaming agent to get phosphoric acid.
In the present embodiment the preparation method of polyether monol, polyether Glycols, polyether-tribasic alcohol and polyethers tetrahydroxylic alcohol with
Embodiment 1 is identical.
Embodiment 5
A kind of dedicated defoaming agent of phosphoric acid processing is present embodiments provided, 30 parts of polyether monol is weighed in parts by weight, gathers
0.5 part of 30 parts of ether dihydric alcohol, 20 parts of polyether-tribasic alcohol, 5 parts of polyethers tetrahydroxylic alcohol, 1 part of soybean oil, 3 parts of sapn and tween addition are stirred
It mixes in tank, is stirred evenly under conditions of 80 DEG C and process dedicated defoaming agent to get phosphoric acid.
In the present embodiment the preparation method of polyether monol, polyether Glycols, polyether-tribasic alcohol and polyethers tetrahydroxylic alcohol with
Embodiment 2 is identical.
Embodiment 6
A kind of dedicated defoaming agent of phosphoric acid processing is present embodiments provided, 20 parts of polyether monol is weighed in parts by weight, gathers
1 part of 35 parts of ether dihydric alcohol, 25 parts of polyether-tribasic alcohol, 10 parts of polyethers tetrahydroxylic alcohol, 3 parts of soybean oil, 2 parts of sapn and tween addition stirring
In tank, is stirred evenly under conditions of 80 DEG C and process dedicated defoaming agent to get phosphoric acid.
In the present embodiment the preparation method of polyether monol, polyether Glycols, polyether-tribasic alcohol and polyethers tetrahydroxylic alcohol with
Embodiment 3 is identical.
Comparative example 1
A kind of phosphoric acid processes dedicated defoaming agent, weigh in parts by weight 35 parts of polyether Glycols, 25 parts of polyether-tribasic alcohol and
In 10 parts of addition agitator tanks of polyethers tetrahydroxylic alcohol, is stirred evenly under conditions of 80 DEG C and process dedicated defoaming agent to get phosphoric acid.
In this comparative example, preparation method and 3 phase of embodiment of polyether Glycols, polyether-tribasic alcohol and polyethers tetrahydroxylic alcohol
Together.
Comparative example 2
A kind of phosphoric acid processes dedicated defoaming agent, weigh in parts by weight 20 parts of polyether monol, 25 parts of polyether-tribasic alcohol and
In 10 parts of addition agitator tanks of polyethers tetrahydroxylic alcohol, is stirred evenly under conditions of 80 DEG C and process dedicated defoaming agent to get phosphoric acid.
In this comparative example, preparation method and 3 phase of embodiment of polyether monol, polyether-tribasic alcohol and polyethers tetrahydroxylic alcohol
Together.
Comparative example 3
A kind of phosphoric acid processes dedicated defoaming agent, weigh in parts by weight 20 parts of polyether monol, 35 parts of polyether Glycols and
In 10 parts of addition agitator tanks of polyethers tetrahydroxylic alcohol, is stirred evenly under conditions of 80 DEG C and process dedicated defoaming agent to get phosphoric acid.
In this comparative example, preparation method and 3 phase of embodiment of polyether monol, polyether Glycols and polyethers tetrahydroxylic alcohol
Together.
Comparative example 4
A kind of phosphoric acid processes dedicated defoaming agent, weigh in parts by weight 20 parts of polyether monol, 35 parts of polyether Glycols and
In 25 parts of addition agitator tanks of polyether-tribasic alcohol, is stirred evenly under conditions of 80 DEG C and process dedicated defoaming agent to get phosphoric acid.
In this comparative example, preparation method and 3 phase of embodiment of polyether monol, polyether Glycols and polyether-tribasic alcohol
Together.
Test example
Performance verification is carried out in order to prove that the performance spy of defoaming agent makees following test:
Expanding foam solution is done with rock phosphate in powder extraction slurry, after pH value is adjusted to 1.0,100mL is contained into accurate calibration
It in the flat graduated cylinder of 600mL, is covered tightly and is clipped on 90 DEG C of vibrating machines with bottle stopper and carry out 100 oscillations, guarantee that foam rises full in graduated cylinder,
It is removed rapidly after oscillation, carries out brokenly bubble and suds suppressing properties evaluation immediately.
1) brokenly bubble performance evaluation: quantitative defoaming agent is accurately equably added to graduated cylinder upper port with dropper, adds rear horse
Upper unlatching stopwatch, the bubble for recording different time in time is high, and each sample is repeated 3 times in parallel.It calculates it and steeps high average value conduct
The standard of defoaming agent performance evaluation steeps Gao Yuegao, illustrates that the brokenly bubble performance of the defoaming agent is poorer, conversely, brokenly bubble performance is better.
2) suds suppressing properties are evaluated: the high each sample of bubble recorded at that time is repeated 3 times in parallel, is calculated it and is steeped high average value work
For the standard of defoaming agent antifoaming ability evaluation, Gao Yuegao is steeped, illustrates that the suds suppressing properties of the defoaming agent are poorer, on the contrary it is better.
1. defoaming agent performance verification result of table
As seen from the above table, the suds suppressing properties of embodiment 4 to 6 and brokenly bubble performance are better than embodiment 1 to 3, embodiment 1 to 3
Suds suppressing properties and brokenly bubble performance be significantly better than embodiment 4 to 6.It can be seen that polyether monol, polyether Glycols, polyethers three
The pure and mild polyethers tetrahydroxylic alcohol of member has synergistic effect to defoaming and foam inhibition；Soybean oil, sapn and tween can be enhanced polyether monol,
The defoaming and foam-inhibiting effect of polyether Glycols, polyether-tribasic alcohol and polyethers tetrahydroxylic alcohol.
Above the embodiments of the present invention are described in detail, but the present invention is not limited to described embodiments.It is right
For those skilled in the art, in the case where not departing from the principle of the invention and spirit, these embodiments are carried out more
Kind change, modification, replacement and modification, still fall in protection scope of the present invention.
Claims (8)
1. a kind of phosphoric acid processes dedicated defoaming agent, which is characterized in that it forms the raw material including following parts by weight: polyethers unitary
10~30 parts of alcohol, 30~40 parts of polyether Glycols, 20~30 parts of polyether-tribasic alcohol and 5~10 parts of polyethers tetrahydroxylic alcohol；The polyethers
The molecular weight of monohydric alcohol is 1000~1500, general formula C4H9O(C3H6O)a(C2H4O)bH；The molecular weight of the dihydric alcohol is 2000
~3000, general formula isThe molecular weight of the polyether-tribasic alcohol is 3000~3600, is led to
Formula isThe molecular weight of the polyethers tetrahydroxylic alcohol is 4000~5000, and general formula is C [CH2O
(C3H6O)n(C2H4O)mH]4。
2. phosphoric acid according to claim 1 processes dedicated defoaming agent, which is characterized in that the preparation side of the polyether monol
Method are as follows: by butanol, the propylene oxide that parts by weight are 100 parts and parts by weight that parts by weight are 5~10 parts be 0.5~1 part
Potassium hydroxide reaction kettle is added, stirring is warming up to 120~130 DEG C, is pressurized to 0.85~0.95MPa, reacts 8~12h；Then
The ethylene oxide that parts by weight are 2~30 parts is added, under conditions of temperature is 90~110 DEG C, pressure is 0.4~0.6MPa,
React 6~10h；3~10h of constant temperature aging under conditions of 90~100 DEG C；Temperature be 100~110 DEG C, vacuum degree be-
It is vacuumized under conditions of 500mmHg~-900mmHg, obtains thick polyether monol；Under conditions of 120~140 DEG C, to thick polyethers
The oxalic acid that parts by weight are 0.5~1 part is added in monohydric alcohol to neutralize, adds the active carbon that parts by weight are 1~5 part and is taken off
Color obtains polyether monol through plate and frame filter press filters pressing under conditions of pressure is 0.3MPa after decoloration.
3. phosphoric acid according to claim 1 processes dedicated defoaming agent, which is characterized in that the preparation side of the polyether Glycols
Method are as follows: be by propylene glycol, the propylene oxide that parts by weight are 90~100 parts and parts by weight that parts by weight are 10~15 parts
Reaction kettle is added in 0.5~1 part of potassium hydroxide, and stirring is warming up to 100~130 DEG C, is pressurized to 0.8~0.9MPa, and reaction 8~
12h；Then it is 10~30 parts of ethylene oxide that parts by weight, which are added, temperature is 90~120 DEG C, pressure is 0.2~0.5MPa
Under conditions of, react 6~10h；It is 3~10h of constant temperature aging in 120~130 DEG C of conditions；It is 100~110 DEG C, very in temperature
Reciprocal of duty cycle vacuumizes under conditions of being -500~-800mmHg, obtains thick polyether Glycols；Under conditions of 110~120 DEG C, gather to thick
The oxalic acid that parts by weight are 0.5~1 part is added in ether dihydric alcohol to neutralize, adds the active carbon that parts by weight are 1~5 part and carries out
Decoloration obtains polyether Glycols through plate and frame filter press filters pressing under conditions of pressure is 0.2MPa after decoloration.
4. phosphoric acid according to claim 1 processes dedicated defoaming agent, which is characterized in that the preparation side of the polyether-tribasic alcohol
Method are as follows: by glycerol, the propylene oxide that parts by weight are 80~100 parts and parts by weight that parts by weight are 15~25 parts be 0.5
Reaction kettle is added in~1 part of potassium hydroxide, and stirring is warming up to 110~150 DEG C, is pressurized to 0.8~0.95MPa, reacts 8~12h；
Then the ethylene oxide that parts by weight are 5~40 parts is added, is 110~120 DEG C in temperature, pressure is the item of 0.2~0.5MPa
Under part, 6~10h is reacted；It is 3~10h of constant temperature aging in 100~120 DEG C of condition of temperature；It is 100~130 DEG C, very in temperature
Reciprocal of duty cycle vacuumizes under conditions of being -500~-800mmHg, obtains thick polyether-tribasic alcohol；Under conditions of 100~130 DEG C, gather to thick
The oxalic acid that parts by weight are 0.5~1 part is added in ether trihydroxylic alcohol to neutralize, adds the active carbon that parts by weight are 1~5 part and carries out
Decoloration obtains polyether-tribasic alcohol through plate and frame filter press filters pressing under conditions of pressure is 0.2MPa after decoloration.
5. phosphoric acid according to claim 1 processes dedicated defoaming agent, which is characterized in that the preparation side of the polyethers tetrahydroxylic alcohol
Method are as follows: be by pentaerythrite, the propylene oxide that parts by weight are 80~120 parts and parts by weight that parts by weight are 10~15 parts
Reaction kettle is added in 0.5~1 part of potassium hydroxide, and stirring is warming up to 90~110 DEG C, is pressurized to 0.8~1MPa, reacts 8~12h；
Then the ethylene oxide that parts by weight are 0~40 part is added, in the item that temperature is 110~130 DEG C, pressure is 0.2~0.3MPa
Under part, 6~10h is reacted；3~10h of constant temperature aging under conditions of 130~140 DEG C；It is 100~110 DEG C, vacuum degree in temperature
To vacuumize under conditions of -500~-800mmHg, thick polyethers tetrahydroxylic alcohol is obtained；Under conditions of 100~110 DEG C, to thick polyethers four
The oxalic acid that parts by weight are 0.5~1 part is added in first alcohol to neutralize, adds the active carbon that parts by weight are 1~5 part and is taken off
Color obtains polyethers tetrahydroxylic alcohol through plate and frame filter press filters pressing under conditions of pressure is 0.3MPa after decoloration.
6. phosphoric acid according to claim 1 processes dedicated defoaming agent, which is characterized in that further include parts by weight be 1~5 part
Soybean oil, the sapn that parts by weight are 1~3 part and the tween that parts by weight are 0.5~2 part.
7. a kind of processing method that the described in any item phosphoric acid of Claims 1 to 5 process dedicated defoaming agent, which is characterized in that press
Parts by weight weigh polyether monol, polyether Glycols, polyether-tribasic alcohol and polyethers tetrahydroxylic alcohol and are added in agitator tank, 70~80
It is stirred evenly under conditions of DEG C and processes dedicated defoaming agent to get the phosphoric acid.
8. a kind of processing method that phosphoric acid as claimed in claim 6 processes dedicated defoaming agent, which is characterized in that claim in parts by weight
Polyether monol, polyether Glycols, polyether-tribasic alcohol, polyethers tetrahydroxylic alcohol, soybean oil, sapn and tween is taken to be added in agitator tank,
It is stirred evenly under conditions of 70~80 DEG C and processes dedicated defoaming agent to get the phosphoric acid.
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