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CN1158836A - Refined glycerine prepared with fermented glycerine solution and its refinement process and equipment - Google Patents

Refined glycerine prepared with fermented glycerine solution and its refinement process and equipment Download PDF

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Publication number
CN1158836A
CN1158836A CN 96115672 CN96115672A CN1158836A CN 1158836 A CN1158836 A CN 1158836A CN 96115672 CN96115672 CN 96115672 CN 96115672 A CN96115672 A CN 96115672A CN 1158836 A CN1158836 A CN 1158836A
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communicated
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glycerine
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glycerol
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CN 96115672
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王瑞梅
王勇
陈萃花
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Abstract

The present invention produces glycerine with purity over 98.5%. The refining process includes the mechanical method eliminating suspended yeast in fermented solution; the ion exchange method eliminating anion, cation, pigment, saccharide and other impurities; and finally, the physico-chemical method including evaporating concentration of filtrate glycerine, rectification and active decoloring. The special equipment includes three sets: centrifugal separator, plate-frame filter and filtrator for eliminating suspension; four ion exchange columns with three kinds of resin for the ion exchange process; and counter-current three-effect evaporator, rectifying tower, decoloring cylinder and automatic filtrator for the final process.

Description

Glycerol fermentation fermented glycerine solution and process for purification thereof and specific equipment
The invention belongs to organic applied chemistry field, particularly be to produce refining glycerine and process for purification and specific equipment the glycerol fermented broth of glycerine from fermentation method.
Glycerine is a kind of general industrial chemicals of having many uses, and the product with fermentative Production glycerine goes on the market at present.The existing operational path that extracts the glycerine employing from glycerol fermented broth is: fermented liquid concentrates after centrifuging, glycerol content is reached about 80%, add again that absorption carrier (as carclazyte) distills, fractional condensation, obtain glycerine and sugar water, raw glycerine is used activated carbon decolorizing again, use the flame filter press press filtration again, obtain product glycerine.The shortcoming that existing fermentation method is produced glycerine is: product glycerine of poor quality, the complicated component of the organic impurity in the product, and it is unstable, consume highly, the glycerine loss is big, can not continuous production, production efficiency is low, the purity of product is the highest can only to be reached about 95%, and the required glycerine of domestic food and medical department is still by import.There are three families the Shandong Province at present, and the quality of more than 20 the producer's fermentative Production glycerine in the whole nation all reaches the not standard of medicine food level, is in predicament, if product purity is reached more than 98%, with regard to energy import substitution product, also there has been outlet in domestic manufacturer.
The purpose of this invention is to provide a kind of purification of glycerin technology that can overcome above-mentioned shortcoming, to the suspended substance in the glycerol fermented broth, zwitterion reaches and can show electropositivity or electronegative macro-radical (or compound), aldehyde or second compound that carbon is ketone group under electrostatic field, separate away with water etc. as organic pigments such as glucose, fructose, octenals, reach pharmaceutical grade, food grade refining glycerine and process for purification and specific equipment more than 98.5% thereby obtain purity.
The object of the present invention is achieved like this, and accompanying drawings is as follows:
A kind of process for purification of glycerol fermentation fermented glycerine solution, its technical process is:
1. earlier remove yeast suspension thing in the glycerol fermented broth with mechanical process;
2. remove impurity such as zwitterion in the glycerol fermented broth, pigment, carbohydrate with ion exchange method again and obtain the glycerol fermentation clear filtrate;
3. with physico-chemical method the glycerine clear filtrate is carried out evaporation concentration, rectifying, decolours, removes its solvability impurity at last, obtain refining glycerine;
4. the glycerine purity of this kind method acquisition reaches more than 98.5%.
The process for purification of above-mentioned glycerol fermentation fermented glycerine solution, wherein the suspended substance that removes in the glycerol fermented broth of mechanical process is meant: with glycerol fermented broth from fermentor tank 101, separate, filter, remove suspended substance wherein by whizzer 103, pressure filter 106, efficient board-like all filters 109 successively, make the glycerol fermentation clear filtrate, its clear filtrate fineness is 5-10 μ m.
The process for purification of above-mentioned glycerol fermentation fermented glycerine solution, wherein ion exchange method is meant: utilize strongly basic anionic resin D201, Subacidity cation 122 and contain primary amine groups because of weakly-basic anion D302 or three kinds of resins of D303, respectively in placed in-line resin-column (202), (203) and the exchange column A (206) that is together in series, B (207), cooperatively interacting removes zwitterion, pigment, carbohydrate in the glycerol fermented broth.
The processing condition that the process for purification intermediate ion switching technology of above-mentioned glycerol fermentation fermented glycerine solution removes zwitterion pigment, carbohydrate are:
1. temperature 10-80 ℃;
②PH=3-14;
3. decolouring and breaking away from sub-air speed is 0.2-10[hour] -1, got 0.5-4[hour] -1Best;
4. desugar air speed is 0.1-5[hour] -1, got 0.2-2[hour] -1Best;
5. desugar can adopt one or more levels, secondary, three grades of best results.
Physico-chemical method in the process for purification of above-mentioned glycerol fermentation fermented glycerine solution to the glycerol fermentation clear filtrate that makes evaporate, concentrate, the technological process and the condition of rectifying, purification be:
1. used equipment is: triple-effect evaporator I (302), II (304), III (306) and rectifying tower (309), condenser (311), bleacher (314) and all filters (316) of efficient board-like airtight automatic sludge discharge;
2. vacuum concentration can adopt single-action/triple-effect evaporator (302), (304), (306), and its temperature is 40-80 ℃, and pressure is 60-700mmHg;
3. the rectifying of rectifying tower (309) is carried out continuously, and its temperature is 110-210 ℃, and pressure is 10-60mmHg;
4. active carbon for decolorization is at bleacher (314) secondary decolourization, and with efficient board-like airtight automatic sludge discharge week filter (316), fineness is 5-10 μ m, obtains refining glycerine after the filtration.
The specific equipment that a kind of process for purification of above-mentioned glycerol fermentation fermented glycerine solution is used, its constructional feature is:
1. be divided into three units in a whole set of specific equipment successively:
First group is that machinery removes the suspended substance unit;
Second group is that ion exchange column removes zwitterion, pigment, carbohydrate unit;
The 3rd group is evaporation concentration, rectifying, decolorization and purification unit;
2. be communicated with by pipeline successively between three units.
Accompanying drawing is the specific equipment structural representation of glycerol fermentation fermented glycerine solution.
Description of drawings and embodiment:
In conjunction with the accompanying drawings to foregoing machinery remove the suspended substance unit both the equipment of first unit and annexation further specify into:
Glycerol fermentation jar 101 outlets passing through fermentation liquid pump 102 is communicated with the left side of yeast separator 103 is suitable for reading, and the magma transferpump 105 that the left side of yeast separation machine 103 exports down by magma groove 104 and connection thereof is communicated with the inlet of plate and frame(type)filter press 106; The right side of aforementioned yeast separator 103 outlet down is communicated with the inlet of thin liquid groove 107 simultaneously with plate and frame(type)filter press 106 outlets; The outlet of thin liquid groove 107 is communicated with the lower-left side outlet of all filters 109 by thin liquid transferpump 108, and the right side outlet of all filters 109 is communicated with the inlet of clear filtrate transferpump 201 by clear filtrate groove 110;
In conjunction with the accompanying drawings aforementioned ion exchange column is removed zwitterion, pigment and carbohydrate the unit both equipment and the annexation that comprise of second unit further specify as follows: the outlet of clear filtrate transferpump 201 is communicated with the upper inlet of strong base anion resins post 202, it exports down and is communicated with the upper inlet of low-acid cationic resin post 203, the following outlet of low-acid cationic resin post 203 is communicated with the upper inlet of desugar ion exchange column 206 by destainer groove 204 and destainer transferpump 205, it exports down and is communicated with the upper inlet of desugar ion exchange column 207, and the following outlet of desugar ion exchange column B207 is communicated with by the inlet of decolouring liquid glucose groove 208 with decolouring desugar liquid transferpump 301;
In conjunction with the accompanying drawings to aforesaid evaporation, concentrate, rectifying, decolorization and purification unit both included equipment and the annexation of the 3rd unit is described as follows: the outlet of decolouring desugar liquid transferpump 301 is communicated with the sidewall inlet of triple-effect evaporator I302, outlet is communicated with the side inlet of triple-effect evaporator II304 by one-level concentrate pump 303 again below the sidewall of three vaporizer I302, triple effect evaporation is communicated with the side inlet of triple-effect evaporator III306 by secondary concentrate pump 305 along the side exit of II304 again, the side exit of triple-effect evaporator III306 is communicated with the side inlet of rectifying tower 309 by concentrated solution transferpump 308 again, the upper outlet of rectifying tower 309 is communicated with the upper inlet of condenser 311, the following outlet of condenser 311 is communicated with the upper inlet of bleacher 314 by raw glycerine groove 312 and raw glycerine transferpump 313, the following outlet of bleacher 314 is communicated with the side lower inlet of all filters 316 by decolouring material conveying pump 315, and the side of all filters 316 is suitable for reading to be the outlet of refining glycerine.
Triple-effect evaporator I302, II304 and III306 in the above-mentioned evaporation rectifying unit all have chuck; The Jacket inlet 317 of triple-effect evaporator III306 is the heating steam inlet, suitable for readingly in the III306 be communicated with the Jacket inlet of II304, upper outlet in the II304 is communicated with the Jacket inlet of I302, the upper outlet of last triple-effect evaporator I302 is communicated with the inlet of the condenser 307 that vacuum system is ined succession, and the outlet of condenser 307 is the condensing air outlet.
The following outlet of above-mentioned rectifying tower 309 is communicated with rectifying tower 309 side inlets by still liquid recycle pump 310.
Communicating pipe should connect the threeway tube head between above-mentioned raw glycerine transferpump 313 and bleacher 314 inlets, its another tube head is communicated with rectifying tower 309 side inlets.
Embodiment: (1) mechanical process removes suspended substances such as yeast
Contain a large amount of zymic yellowish brown glycerol fermented broths in the glycerol fermentation jar 101, enter in the yeast separator 103 by fermentation liquid pump 102 and separate, enter magma groove 104 again, enter plate and frame(type)filter press 106 press filtrations by magma transferpump 105; Gained yeast filter cake can be sold, and filtrate and all enter thin liquid groove 107 by isolated clear liquid in the whizzer 103 is got in efficient board-like airtight automatic sludge discharge week filter 109 by thin liquid transferpump 108 again, and the slag that filters out also can be sold; Clear liquid enters groove 110, finish the operation that machinery removes suspended substance this moment, in the wherein efficient board-like airtight automatic sludge discharge week filter, form with self or filter by the filter membrane that diatomite forms, filtering fineness is 5-10 μ m, and obtaining clear filtrate is the liquid of the yellow orange of little apparent muddiness.
(2) remove zwitterion, pigment and carbohydrate with ion exchange method:
1. take off the ionic liquid preparation:
The above-mentioned glycerol fermentation filtrate that makes of 20Kg is squeezed into from filtrate groove 110 in the strong base anion resins post 202 that contains D201 through transferpump 201, enter again and contain in 122 the acidulous cation resin post 203, requirement evenly by 4.8 liters D201 negative resin and 4.8 122 positive resins, almost was water white aqueous glycerin solution in 4 hours;
2. the preparation of desugar liquid:
With above-mentioned destainer with the flow velocity of 40ml per hour uniformly by 50mlD302 weak base anion-exchange resin post A206 and ion exchange column B207, can not check glucose in the resulting desugar liquid.
(3) evaporation, concentrate, rectifying produces the glycerine more than 98.5%:
With the water white aqueous glycerin solution of the above-mentioned decolouring that obtains, desugar squeeze into adverse current triple-effect evaporator I302, II (304) successively, III (306) is 60 ℃ with temperature, pressure is that 200mmHg carries out evaporation concentration, squeeze into rectifying tower 309 again behind the content of minimizing water, with pressure 50mmHg, temperature is 180 ℃ and carries out continuous rectification, further use the gac secondary decolourization again, and with efficient board-like airtight automatic sludge discharge filter 316, fineness is filtered and is obtained the refining glycerine of purity more than 98.5% less than 8 μ m.
Advantage of the present invention has a lot, because in the design at first is to remove suspended substance with mechanical means, remove the various zwitterions that form in the residual sugar (as glucose) that reacts and the biological process, pigment etc. with ion exchange adsorption, it is unique especially especially to select for use D302 and D303 to contain the anionite-exchange resin desugar of primary amine group; Further separate purification with reduction vaporization, rectifying, activated carbon decolorizing, improved the quality of fermentation method glycerine, improved yield, reduced consumption, reduced cost, solved the problem that refining purification that fermentation method glycerine faced does not pass a test.By method provided by the present invention and specific equipment, satisfy the specification of quality of industries such as medicine, food, polyethers, paint fully.

Claims (10)

1, a kind of process for purification of glycerol fermentation fermented glycerine solution is characterized in that:
1. earlier remove yeast suspension thing in the glycerol fermented broth with mechanical process;
2. remove impurity such as zwitterion in the glycerol fermented broth, pigment, carbohydrate with ion exchange method again and obtain the glycerol fermentation clear filtrate;
3. with physico-chemical method the glycerine clear filtrate is carried out evaporation concentration, rectifying, decolours, removes its solvability impurity at last, obtain refining glycerine;
4. the glycerine purity of this kind method acquisition reaches more than 98.5%.
2, the process for purification of glycerol fermentation fermented glycerine solution according to claim 1, it is characterized in that: wherein the suspended substance that removes in the glycerol fermented broth of mechanical process is meant: with glycerol fermented broth from fermentor tank 101, separate, filter, remove suspended substance wherein by whizzer 103, pressure filter 106, efficient board-like all filters 109 successively, make the glycerol fermentation clear filtrate, its clear filtrate fineness is 5-10 μ m.
3, the process for purification of glycerol fermentation fermented glycerine solution according to claim 1, it is characterized in that: wherein ion exchange method is meant: utilize strongly basic anionic resin D201, Subacidity cation 122 and contain primary amine groups because of weakly-basic anion D302 or three kinds of resins of D303, respectively in placed in-line resin-column (202), (203) and the exchange column A (206) that is together in series, B (207), cooperatively interacting removes zwitterion, pigment, carbohydrate in the glycerol fermented broth.
4, the process for purification of glycerol fermentation fermented glycerine solution according to claim 3 is characterized in that: the processing condition that ion exchange method removes zwitterion, pigment, carbohydrate are:
1. temperature 10-80 ℃;
②PH=3-14;
3. decolouring and breaking away from sub-air speed is 0.2-10[hour] -1, got 0.5-4[hour] -1Best;
4. desugar air speed is 0.1-5[hour] -1, got 0.2-2[hour] -1Best;
5. desugar can be adopted one or more levels; Secondary, three grades of best results.
5, the process for purification of glycerol fermentation fermented glycerine solution according to claim 1 is characterized in that: described physico-chemical method to the glycerol fermentation clear filtrate evaporates, concentrates, rectifying, is meant with activated carbon decolorizing and solvability impurity:
1. used equipment with the pipeline connection is in proper order: triple-effect evaporator I (302), II (304), III (306) and rectifying tower (309), condenser (311), bleacher (314) and all filters (316) of efficient board-like airtight automatic sludge discharge;
2. vacuum concentration can adopt single-action/triple-effect evaporator (302), (304), (306), and its temperature is 40-80 ℃, and pressure is 60-700mmHg;
3. the rectifying of rectifying tower (309) is carried out continuously, and its temperature is 110-210 ℃, and pressure is 10-60mmHg;
4. active carbon for decolorization is at bleacher (314) secondary decolourization, and filters with efficient board-like airtight automatic sludge discharge week filter (316), and fineness is 5-10 μ m, obtains refining glycerine after the filtration.
6, the used specific equipment of a kind of process for purification of glycerol fermentation fermented glycerine solution according to claim 1 is characterized in that:
1. be divided into three units in a whole set of specific equipment successively:
First unit is that machinery removes the suspended substance unit;
Second unit is that ion exchange column removes zwitterion, pigment, carbohydrate unit;
The 3rd unit is evaporation concentration, rectifying, decolorization and purification unit;
2. be communicated with by pipeline successively between three units.
7, the specific equipment of glycerol fermentation fermented glycerine solution according to claim 6 is characterized in that:
First unit equipment and annexation are: fermentor tank (101) exported by left side suitable for reading be communicated with of fermentation liquid pump (102) with yeast separator (103), and the left side of yeast separation machine 103 exports the magma transferpump (105) that passes through magma groove (104) and be communicated with down and is communicated with the inlet of plate and frame(type)filter press (106); The right side of aforementioned yeast separator (103) outlet down is communicated with the inlet of thin liquid groove (107) simultaneously with plate and frame(type)filter press (106) outlet; The outlet of thin liquid groove (107) is communicated with the lower-left side outlet of all filters (109) by thin liquid transferpump (108), and the right side outlet of all filters (109) is communicated with the inlet of clear filtrate transferpump (201) by clear filtrate groove (110);
Second unit equipment and annexation are: the outlet of clear filtrate transferpump (201) is communicated with the upper inlet of strong base anion resins post (202), it exports down and is communicated with the upper inlet of low-acid cationic resin post (203), the following outlet of low-acid cationic resin post (203) is communicated with the upper inlet of desugar ion exchange column A (206) by destainer groove (204) and destainer transferpump (205), it exports down and is communicated with the upper inlet of desugar ion exchange column B (207), and the following outlet of desugar ion exchange column B (207) is communicated with by the inlet of decolouring liquid glucose groove (208) with decolouring desugar liquid transferpump (301);
The 3rd unit equipment and annexation are: the outlet of decolouring desugar liquid transferpump (301) is communicated with the sidewall of triple-effect evaporator I (302) inlet, outlet is communicated with the side inlet of triple-effect evaporator II (304) by one-level concentrate pump (303) again below the sidewall of three vaporizer I (302), triple effect evaporation is communicated with the side inlet of triple-effect evaporator III (306) by secondary concentrate pump (305) along the side exit of II (304) again, the side exit of triple-effect evaporator III (306) is communicated with the side inlet of rectifying tower (309) by concentrated solution transferpump (308) again, the upper outlet of rectifying tower (309) is communicated with the upper inlet of condenser (311), the following outlet of condenser (311) is communicated with the upper inlet of bleacher (314) by raw glycerine groove (312) and raw glycerine transferpump (313), the following outlet of bleacher (314) is communicated with the side lower inlet of all filters (316) by decolouring material conveying pump (315), and the side of all filters (316) is suitable for reading to be the outlet of refining glycerine.
8, the specific equipment of glycerol fermentation fermented glycerine solution according to claim 7 is characterized in that: the triple-effect evaporator I (302) in the 3rd unit, II (304) and III (306) all have chuck; The Jacket inlet (317) of triple-effect evaporator III (306) is the heating steam inlet, the Jacket inlet with II (304) suitable for reading is communicated with in the III (306), upper outlet in the II (304) is communicated with the Jacket inlet of I (302), the upper outlet of last triple-effect evaporator I (302) is communicated with the inlet of the condenser (307) that vacuum system is ined succession, and the outlet of condenser (307) is the condensing air outlet.
9, the specific equipment of glycerol fermentation fermented glycerine solution according to claim 7 is characterized in that: the following outlet of the rectifying tower in the 3rd unit (309) is communicated with rectifying tower (309) side inlet by still liquid recycle pump (310).
10, the specific equipment of glycerol fermentation fermented glycerine solution according to claim 8, it is characterized in that: communicating pipe should connect the threeway tube head between raw glycerine transferpump (313) and bleacher (314) inlet, its another tube head is communicated with rectifying tower (309) side inlet.
CN 96115672 1996-03-06 1996-03-06 Refined glycerine prepared with fermented glycerine solution and its refinement process and equipment Pending CN1158836A (en)

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Application Number Priority Date Filing Date Title
CN 96115672 CN1158836A (en) 1996-03-06 1996-03-06 Refined glycerine prepared with fermented glycerine solution and its refinement process and equipment

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 96115672 CN1158836A (en) 1996-03-06 1996-03-06 Refined glycerine prepared with fermented glycerine solution and its refinement process and equipment

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CN1158836A true CN1158836A (en) 1997-09-10

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2437516A (en) * 2006-04-26 2007-10-31 Bai Leng Method and apparatus for purifying glycerine using filter membranes and a deionisation means
US7595070B2 (en) 2005-06-21 2009-09-29 The Coca-Cola Company Method for removing contaminants from essential oils
GB2459738A (en) * 2008-05-07 2009-11-11 Bai Leng Purification of glycerine
CN103936554A (en) * 2014-05-05 2014-07-23 龙岩卓越新能源股份有限公司 Two-time glycerol decoloring method
CN105176138A (en) * 2015-10-19 2015-12-23 营口晨光植物提取设备有限公司 Continuous multifunctional water-soluble pigment extraction equipment
CN115745746A (en) * 2022-07-29 2023-03-07 湖北天基生物能源科技发展有限公司 Glycerol refining method

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7595070B2 (en) 2005-06-21 2009-09-29 The Coca-Cola Company Method for removing contaminants from essential oils
GB2437516A (en) * 2006-04-26 2007-10-31 Bai Leng Method and apparatus for purifying glycerine using filter membranes and a deionisation means
GB2459738A (en) * 2008-05-07 2009-11-11 Bai Leng Purification of glycerine
WO2009136181A1 (en) * 2008-05-07 2009-11-12 Bai Leng Method of purification of glycerine
GB2459738B (en) * 2008-05-07 2013-03-06 Bai Leng Method of purification
CN103936554A (en) * 2014-05-05 2014-07-23 龙岩卓越新能源股份有限公司 Two-time glycerol decoloring method
CN103936554B (en) * 2014-05-05 2015-09-23 龙岩卓越新能源股份有限公司 Glycerin secondary decolorization method
CN105176138A (en) * 2015-10-19 2015-12-23 营口晨光植物提取设备有限公司 Continuous multifunctional water-soluble pigment extraction equipment
CN105176138B (en) * 2015-10-19 2016-11-30 营口晨光植物提取设备有限公司 Multifunctional water lysochrome extraction equipment continuously
CN115745746A (en) * 2022-07-29 2023-03-07 湖北天基生物能源科技发展有限公司 Glycerol refining method

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