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CN110614085A - Preparation method of desorption-free adsorbent with large-particle trepanning structure - Google Patents

Preparation method of desorption-free adsorbent with large-particle trepanning structure Download PDF

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Publication number
CN110614085A
CN110614085A CN201910638748.7A CN201910638748A CN110614085A CN 110614085 A CN110614085 A CN 110614085A CN 201910638748 A CN201910638748 A CN 201910638748A CN 110614085 A CN110614085 A CN 110614085A
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parts
adsorbent
desorption
weighing
colloid
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Inventor
苟进锋
骆筱
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Xi'an Hairun New Materials Co Ltd
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Xi'an Hairun New Materials Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12Naturally occurring clays or bleaching earth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/14Diatomaceous earth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26Synthetic macromolecular compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/34Regenerating or reactivating

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Dispersion Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

A preparation method of a desorption-free adsorbent with a large particle trepanning structure comprises the following steps in parts by weight: 1) weighing 5-20 parts of macroporous ion exchange resin, grinding, sieving, adding deionized water into sieved fine-grained powder for wetting, adding sulfuric acid for acidification, and performing ultrasonic activation; 2) adding acid into the inorganic adsorbent and carrying out ultrasonic activation; 3) selecting a proper colloid, adding deionized water to prepare a solution, uniformly mixing the activated products prepared in the step 1) and the step 2), adding the mixture into a mixed solution of the colloid and water, uniformly stirring, and ultrasonically blending; 4) adjusting the ph to be neutral, adding the cultured thalli, uniformly stirring, pouring into a mould for granulation, and drying at low temperature to obtain the porous adsorption material; has the characteristics of low cost and wide application range.

Description

Preparation method of desorption-free adsorbent with large-particle trepanning structure
Technical Field
The invention belongs to the technical field of adsorbents, and particularly relates to a preparation method of a desorption-free adsorbent with a large-particle trepanning structure.
Background
In recent years, with the environmental protection awareness, the work of efficiently treating industrial wastewater is compelling. The adsorption method is capable of removing pollutants without damaging the pollutants, and only accumulates the pollutants on the adsorbent from the polluted water body, so that high-risk intermediate products are not generated. The surface structure of the adsorbent, the molecular structure of the adsorbate, the properties of functional groups, and the like are main factors influencing the adsorption rate, and in conclusion, the research and development of the general adsorbent and the renewable adsorbent are the key points of the application of the adsorption technology. The adsorbent commonly used in the current engineering practice is mainly inorganic adsorption material and organic adsorption resin. The inorganic adsorption material has considerable specific surface area and ultramicro capillary, and has wide application, low price, slow adsorption rate and poor regenerability; the organic adsorption resin has large adsorption capacity and good reproducibility, but the organic adsorption resin has high price, strong selectivity and narrow application range. Therefore, the development of the adsorption material which has wide application range, high adsorption capacity, good reproducibility and moderate price has important significance for green emission of factory wastewater.
Although some researchers have improved the defects of slow adsorption rate and poor regenerability of the inorganic adsorbent and some researchers have adjusted the application range of the adsorbent resin, the regenerable inorganic adsorbent still has the problems of poor regenerability, low adsorption capacity and the like, and the cost of wastewater treatment cannot be reduced due to the limitation of synthetic raw materials of the organic adsorbent resin and the high price.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of a desorption-free adsorbent with a large-particle trepanning structure, which introduces an inorganic adsorption material into adsorption resin, so that the advantages of the two materials are complementary, the effect is exerted, meanwhile, microbial degradation is introduced in the preparation, the procedure is reduced for later desorption regeneration, the self regeneration can be directly realized, the resource waste is not needed, the problems of high cost and narrow application range of the adsorption resin are solved, and the preparation method has the characteristics of low cost and wide application range.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of a desorption-free adsorbent with a large-particle trepanning structure comprises the following steps in parts by weight:
1) weighing 5-20 parts of macroporous ion exchange resin, grinding at a high speed, sieving by a sieve with 90-200 meshes, adding deionized water to wet the sieved fine-grained powder, adding 1-4% sulfuric acid to acidify the powder, and ultrasonically activating the powder for 20-40 min by using a KQ2200E ultrasonic cleaner, wherein the amount of the sulfuric acid is less than that of the powder;
2) weighing 0.7-7 parts of inorganic adsorbent component, and adding sulfuric acid with the amount exceeding that of the solid component for ultrasonic activation for 30 min;
3) weighing 2-8.5 parts of colloid, adding deionized water according to the proportion of 1: 1-1: 20 to prepare a solution, uniformly mixing the activated products prepared in the step 1) and the step 2), adding the activated products into a mixed solution of the colloid and water, uniformly stirring, and ultrasonically blending for 2 hours;
4) and adjusting the ph to be neutral, adding 2-10 parts of cultured thalli, uniformly stirring, pouring into a mold for granulation, and drying at low temperature to obtain the porous adsorbing material.
The macroporous ion exchange resin is any one or mixture of more commercially available macroporous ion exchange resins;
the inorganic adsorbent is one or the combination of any more of active carbon, kaolin, attapulgite, zeolite and diatomite.
The colloid is one or a mixture of any more of polyvinyl alcohol, carboxymethyl cellulose, pure acrylic emulsion, styrene-acrylic emulsion, silicone-acrylic emulsion and VAE emulsion.
The thallus is one of bacillus, serratia and neisseria.
Compared with the prior art, the invention has the beneficial effects that:
1) the adsorption range is wide, the advantages of organic and inorganic adsorption are achieved, and the required shape and size can be molded by replacing the mold according to the use requirement.
2) The introduction of active bacteria can directly reduce the adsorbed substances in the adsorbent body without desorption and regeneration.
3) The invention aims to solve the problems of high cost and narrow application range of the adsorption resin. The inorganic adsorption material is introduced into the adsorption resin, so that the advantages of the two materials are complementary and the effect is exerted; meanwhile, microbial degradation is introduced in the preparation, so that the procedure is reduced for later desorption regeneration, the regeneration can be directly carried out, and the resource waste is not needed.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
Weighing 8 parts of commercially available D301 macroporous anion exchange resin, grinding by a high-speed grinder, sieving by a 160-mesh sieve, wetting sieved powder by deionized water, and adding 2% sulfuric acid to activate in ultrasound for 30 min; simultaneously weighing 1 part of activated carbon, and performing ultrasonic activation for 30min by using 2% sulfuric acid; weighing 5 parts of VAE emulsion and 11 parts of deionized water, uniformly stirring, uniformly mixing the two activated powders, adding the mixture into a mixed solution of colloid and water, uniformly stirring, and ultrasonically blending for 2 hours; and adjusting the ph to be neutral, adding 3 parts of cultured bacillus, uniformly stirring, pouring into a mould for granulation, and drying at low temperature to obtain the porous adsorption material.
Example 2
Weighing 6 parts of commercially available D401 chelating resin and 4 parts of D100 anionic resin, respectively grinding by a high-speed grinder, sieving by a 90-mesh sieve, mixing, wetting sieved powder by deionized water, adding 4% sulfuric acid, and activating for 20min in ultrasonic; simultaneously weighing 3 parts of activated carbon and 4 parts of kaolin, and performing ultrasonic activation for 30min by using 4% sulfuric acid; weighing 4 parts of pure acrylic emulsion, 100001.5 parts of polyvinyl alcohol and 30 parts of deionized water, uniformly stirring, uniformly mixing the two activated powders, adding the mixture into a mixed solution of colloid and water, uniformly stirring, and ultrasonically blending for 2 hours; adjusting the pH to be neutral, adding 4 parts of cultured serratia, uniformly stirring, pouring into a mould for granulation, and drying at low temperature to obtain the porous adsorption material.
Example 3
Weighing 20 parts of commercially available 201 multiplied by 7, grinding by a high-speed grinder, sieving by a 180-mesh sieve, mixing, wetting the sieved powder by deionized water, and adding 4% sulfuric acid to activate for 20min in ultrasonic; meanwhile, weighing 7 parts of diatomite, and ultrasonically activating for 30min by using 4% sulfuric acid; weighing 80008.5 parts of polyvinyl alcohol and 28 parts of deionized water, uniformly stirring, uniformly mixing the two activated powders, adding the mixture into a mixed solution of colloid and water, uniformly stirring, and ultrasonically blending for 2 hours; adjusting the pH to be neutral, adding 5 parts of cultured serratia, uniformly stirring, pouring into a mould for granulation, and drying at low temperature to obtain the porous adsorption material.
Example 4
Weighing 14 parts of commercially available 001 x 8IR, grinding by a high-speed grinder, sieving by a 145-mesh sieve, mixing, wetting the sieved powder with deionized water, adding 1% sulfuric acid, and activating for 40min by ultrasound; simultaneously weighing 0.7 part of attapulgite, and ultrasonically activating for 40min by using 1% sulfuric acid; weighing 8.5 parts of sodium carboxymethylcellulose and 32 parts of deionized water, uniformly stirring, uniformly mixing the two types of activated powder, adding the mixture into a mixed solution of colloid and water, uniformly stirring, and ultrasonically blending for 2 hours; adjusting pH to be neutral, adding 2 parts of cultured Neisseria, stirring uniformly, pouring into a die for granulation, and drying at low temperature to obtain the porous adsorption material.
Example 5
Weighing 20 parts of commercially available 201 multiplied by 7, grinding by a high-speed grinder, sieving by a 180-mesh sieve, mixing, wetting the sieved powder by deionized water, and adding 4% sulfuric acid to activate for 20min in ultrasonic; meanwhile, weighing 7 parts of diatomite, and ultrasonically activating for 30min by using 4% sulfuric acid; weighing 80008.5 parts of polyvinyl alcohol and 28 parts of deionized water, uniformly stirring, uniformly mixing the two activated powders, adding the mixture into a mixed solution of colloid and water, uniformly stirring, and ultrasonically blending for 2 hours; adjusting the pH to be neutral, adding 4 parts of cultured serratia, uniformly stirring, pouring into a mould for granulation, and drying at low temperature to obtain the porous adsorption material.
Example 6
Weighing 5 parts of commercially available D318 and 5 parts of commercially available D202, grinding by a high-speed grinder, sieving by a 90-mesh sieve, mixing, wetting sieved powder by deionized water, adding 4% sulfuric acid, and activating for 40min in ultrasonic waves; simultaneously weighing 1 part of kaolin and 1 part of zeolite, and performing ultrasonic activation for 30min by using 4% sulfuric acid; weighing 8 parts of styrene-acrylic emulsion and 13 parts of deionized water, uniformly stirring, uniformly mixing the two activated powders, adding the mixture into a mixed solution of colloid and water, uniformly stirring, and ultrasonically mixing for 2 hours; adjusting the pH to be neutral, adding 3 parts of cultured serratia, uniformly stirring, pouring into a die for granulation, and drying at low temperature to obtain the porous adsorption material.
Example 7
Weighing 8 parts of commercially available D002, grinding by a high-speed grinder, sieving by a 200-mesh sieve, mixing, wetting the sieved powder by deionized water, and adding 4% sulfuric acid to activate for 30min in ultrasonic; meanwhile, weighing 7 parts of diatomite, and ultrasonically activating for 30min by using 4% sulfuric acid; weighing 8 parts of silicone-acrylic emulsion and 8 parts of deionized water, uniformly stirring, uniformly mixing the two types of activated powder, adding the mixture into a mixed solution of colloid and water, uniformly stirring, and ultrasonically blending for 2 hours; adjusting the pH to be neutral, adding 8 parts of cultured serratia, uniformly stirring, pouring into a mould for granulation, and drying at low temperature to obtain the porous adsorption material.
Example 8
Weighing 8 parts of commercially available D002, grinding by a high-speed grinder, sieving by a 200-mesh sieve, mixing, wetting the sieved powder by deionized water, and adding 3% sulfuric acid to activate for 30min in ultrasonic; simultaneously weighing 4.2 parts of zeolite, and ultrasonically activating for 30min by using 3% sulfuric acid; weighing 2 parts of silicone-acrylic emulsion and 5 parts of deionized water, uniformly stirring, uniformly mixing the two types of activated powder, adding the mixture into a mixed solution of colloid and water, uniformly stirring, and ultrasonically blending for 2 hours; adjusting the pH to be neutral, adding 10 parts of cultured serratia, uniformly stirring, pouring into a mould for granulation, and drying at low temperature to obtain the porous adsorption material.

Claims (5)

1. A preparation method of a desorption-free adsorbent with a large particle trepanning structure is characterized by comprising the following steps of:
1) weighing 5-20 parts of macroporous ion exchange resin, grinding at a high speed, sieving by a sieve with 90-200 meshes, adding deionized water to wet the sieved fine-grained powder, adding 1-4% sulfuric acid to acidify the powder, and ultrasonically activating the powder for 20-40 min by using a KQ2200E ultrasonic cleaner, wherein the amount of the sulfuric acid is less than that of the powder;
2) weighing 0.7-7 parts of inorganic adsorbent component, and adding sulfuric acid with the amount exceeding that of the solid component for ultrasonic activation for 30 min;
3) weighing 2-8.5 parts of colloid, adding deionized water according to the proportion of 1: 1-1: 20 to prepare a solution, uniformly mixing the activated products prepared in the step 1) and the step 2), adding the mixture into a mixed solution of the colloid and water, uniformly stirring, and ultrasonically blending for 2 hours;
4) and adjusting the ph to be neutral, adding 2-10 parts of cultured thalli, uniformly stirring, pouring into a mould for granulation, and drying at low temperature to obtain the porous adsorbing material.
2. The method for preparing the desorption-free adsorbent with the large particle trepanning structure according to claim 1, wherein the macroporous ion exchange resin is any one or a mixture of several commercially available macroporous ion exchange resins.
3. The method for preparing the desorption-free adsorbent with the large-particle trepanning structure according to claim 1, wherein the inorganic adsorbent is one or a combination of any of activated carbon, kaolin, attapulgite, zeolite and diatomite.
4. The method for preparing the non-desorption adsorbent with the large particle trepanning structure according to claim 1, wherein the colloid is one or a mixture of any more of polyvinyl alcohol, carboxymethyl cellulose, pure acrylic emulsion, styrene-acrylic emulsion, silicone-acrylic emulsion and VAE emulsion.
5. The method for preparing the non-desorption adsorbent with the large-particle trepanning structure according to claim 1, wherein the thallus is one of bacillus, serratia and neisseria.
CN201910638748.7A 2019-07-16 2019-07-16 Preparation method of desorption-free adsorbent with large-particle trepanning structure Pending CN110614085A (en)

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Application publication date: 20191227