CN110835410A - Method for preparing organic silicon resin with energy conservation and emission reduction - Google Patents

Method for preparing organic silicon resin with energy conservation and emission reduction Download PDF

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Publication number
CN110835410A
CN110835410A CN201911021987.4A CN201911021987A CN110835410A CN 110835410 A CN110835410 A CN 110835410A CN 201911021987 A CN201911021987 A CN 201911021987A CN 110835410 A CN110835410 A CN 110835410A
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organic silicon
washing
water
hydrolysis
preparing
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CN201911021987.4A
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胡磊杰
胡孟进
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CHANGZHOU JIANUO ORGANIC SILICON Co Ltd
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CHANGZHOU JIANUO ORGANIC SILICON Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/06—Preparatory processes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds

Abstract

The invention belongs to the field of resin synthesis, and particularly relates to an energy-saving and emission-reducing method for preparing organic silicon resin, wherein in the process of preparing the organic silicon resin, waste acid water discharged after hydrolysis, water washing and water washing separation is neutralized by a neutralizer added with active alkaline substances, and the neutralized hydrolyzed waste acid water is filtered by a filter to discharge salt-containing wastewater; neutralizing the waste acid water discharged by washing with water by using a neutralizer, separating by using a separator, and discharging salt-containing waste water; the waste acid water after washing and separation is neutralized by a neutralizer, and then secondary circulating water separated by a separator is returned to the hydrolysis and washing procedures for recycling; the method greatly reduces the discharge amount of waste brine formed after hydrolysis and washing, and secondary water after washing and separation can be used for hydrolysis and washing procedures for recycling. The process greatly saves the cost of pollution discharge treatment, saves raw material circulating water, and does not influence the performance of the prepared organic silicon resin.

Description

Method for preparing organic silicon resin with energy conservation and emission reduction
Technical Field
The invention belongs to the field of resin synthesis, and particularly relates to a method for preparing organic silicon resin by adopting a hydrolysis internal circulation process.
Background
The organic silicon resin is an important member in the organic silicon material, is different from the linear structure of the organic silicon rubber and the small molecular weight of the silicon oil and the silane, is a three-dimensional net structure, and has the basic properties of the organic silicon material, such as high temperature resistance, low temperature resistance, high insulation, weather resistance, radiation resistance, chemical resistance, hydrophobicity and the like.
The prior preparation method of the organic silicon resin comprises the following processes: firstly, mixing a metered chlorosilane monomer with an aqueous solution containing an organic solvent, carrying out hydrolysis reaction, and washing and separating after the hydrolysis is finished; then the organic silicon resin is obtained after telomerization and concentration adjustment. Among the prior art, all can produce a large amount of waste acid water in the separation process of hydrolysising, washing to and washing, the waste acid water of discharging on the one hand can produce environmental pollution, and on the other hand carries out the manufacturing cost that the aftertreatment also can greatly increased enterprise to the waste acid water of discharging.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a method for preparing organic silicon resin with energy conservation and emission reduction. In the method, in the process of preparing the organic silicon resin, waste acid water discharged after hydrolysis, washing and washing separation is neutralized by a neutralizer added with active alkaline substances, and the neutralized waste acid water is filtered by a filter to discharge salt-containing waste water; neutralizing the waste acid water discharged by washing with water by using a neutralizer, separating by using a separator, and discharging salt-containing waste water; the waste acid water after washing and separation is neutralized by a neutralizer, and then secondary circulating water separated by a separator is returned to the hydrolysis and washing procedures for recycling; the method greatly reduces the discharge amount of waste brine formed after hydrolysis and washing, and secondary water after washing and separation can be used for hydrolysis and washing procedures for recycling.
The invention discloses a method for preparing organic silicon resin by adopting a hydrolysis internal circulation process, which comprises the following specific process steps:
(1) preparing raw materials according to a proportion;
the raw materials for synthesizing the organic silicon resin are as follows:
basic silicone material monomer: monomethyltrichlorosilane (M1), dimethyldichlorosilane (M2), monophenyltrichlorosilane (P1), diphenyldichlorosilane (P2);
wherein, the purity of the methyl trichlorosilane is more than 99 percent;
dimethyldichlorosilane with purity of more than 99.9%;
mono-phenyl trichlorosilane, purity > 99%;
the purity of the diphenyl dichlorosilane is more than 99 percent;
special organosilicon monomer: can be as follows: one or more than one organic silicon monomer material of organic silicon monomer containing double bond group, organic silicon monomer containing active hydrogen or silane coupling agent.
Wherein, the organosilicon monomer containing double bond group is methyl vinyl dichlorosilane, the organosilicon monomer containing active hydrogen is methyl hydrogen dichlorosilane, and the silane coupling agent can be triethoxy silane containing epoxy group, triethoxy silane containing ester group and triethoxy silane containing amino group and acryloyl group, etc. The organic solvent is: ketone, ether or lipid solvents.
In the total organosilicon monomers, the ratio of the number of organic groups R on silicon atoms to the number of silicon atoms, R/Si is 1.0-1.6, the number of phenyl groups accounts for 15-60% of the total number of R, and the mass of the special organosilicon monomers accounts for 10-40% of the total mass of the organosilicon monomers.
The organic solvent may specifically be: cyclohexanone, butanone, ethyl acetate or butyl ether, wherein the amount of the organic solvent is 2-4 times of the mass of the water;
the water amount is 1-2 times of the total mass of the organic silicon monomer.
(2) Hydrolysis: fully mixing the organic silicon monomers in proportion, and then adding the mixture into an organic solvent for co-hydrolysis;
the cohydrolysis temperature is 4-10 ℃.
Feeding the waste acid water generated by hydrolysis into a neutralizer added with active alkaline substances for neutralization, and filtering and discharging salt-containing wastewater through a filter;
(3) and after the hydrolysis is finished, washing with water, separating by washing with water, then adding a catalyst for telomerization and polycondensation, adding a regulator to reduce the degree of gelation, and regulating the mass fraction of the silicone resin solution to 50% to obtain the silicone resin.
And feeding the waste acid water discharged by washing into a neutralizer added with active alkaline substances for neutralization, separating by a separator, discharging salt-containing wastewater, feeding the waste acid water separated by washing into the neutralizer added with active alkaline substances for neutralization, and returning secondary circulating water separated by the separator to the hydrolysis and washing processes for recycling.
Wherein the added catalyst is a transition metal salt catalyst, specifically platinum chloride, cobalt naphthenate, lead acetate or zinc acetate, and the dosage of the catalyst is 1-2 per mill of the total mass of the organosilicon monomer.
The added regulator is organosilicon oligomer with hydroxyl, epoxy or ester group, and the dosage of the organosilicon oligomer is 20-30% of the total mass of the organosilicon monomer.
Wherein the active alkaline substance is strong alkali inorganic base, Lewis base, hydroxylamine or strong alkali ion exchange resin.
Has the advantages that:
(1) completely discharging or treating the waste acid water in the prior art instead of neutralizing the waste acid water discharged after hydrolysis, washing and washing separation by a neutralizer added with active alkaline substances, and filtering and discharging salt-containing wastewater by a filter after neutralizing the hydrolyzed waste acid water; neutralizing the waste acid water discharged by washing with water by using a neutralizer, separating by using a separator, and discharging salt-containing waste water; the waste acid water after washing and separation is neutralized by the neutralizer, and then the secondary circulating water separated by the separator returns to the hydrolysis and washing procedures for recycling, so that the sewage disposal cost is greatly saved, and the raw material circulating water is saved.
(2) The organic silicon resin is prepared by the internal circulation process, the post-treatment of acid water is not needed, only a trace amount of salt-containing wastewater is generated, the requirements of energy conservation and emission reduction are met, and the production cost is reduced.
Drawings
FIG. 1 is a flow chart of the hydrolysis internal circulation process of the present invention.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1
The raw materials for synthesizing the organic silicon resin comprise the following components in percentage by mass:
120 parts of methyltrichlorosilane (M1);
80 parts of dimethyldichlorosilane (M2);
80 parts of phenyltrichlorosilane (P1);
120 parts of diphenyldichlorosilane (P2);
120 parts of ester-containing organosilicon coupling agent.
Fully mixing the organic silicon monomers in proportion, adding the mixture into 600 parts of benzene, adding 1200 parts of butanone and 600 parts of water, controlling the hydrolysis temperature at 5 ℃, completing hydrolysis within 5 hours, performing water washing and water washing separation after the hydrolysis is completed, then adding 1 part of lead naphthenate catalyst, adding 140 parts of epoxy group organic silicon low molecule serving as an adjusting agent, reducing the degree of gelation, then adding toluene, and adjusting the solid content to be 50% solution to obtain the organic silicon resin.
Neutralizing the discharged waste acid water after hydrolysis, water washing and water washing separation by a neutralizer added with active alkaline substances, and filtering and discharging salt-containing wastewater by a filter after the neutralization of the hydrolyzed waste acid water; neutralizing the waste acid water discharged by washing with water by using a neutralizer, separating by using a separator, and discharging salt-containing waste water; the waste acid water after washing and separation is neutralized by a neutralizer, and then secondary circulating water separated by a separator is returned to the hydrolysis and washing processes for recycling.
One ton of resin was produced and the discharge of the brine waste after neutralization after separation was only 4 tons.
Example 2
The raw materials for synthesizing the organic silicon resin comprise the following components in percentage by mass:
110 parts of methyltrichlorosilane (M1);
60 parts of dimethyldichlorosilane (M2);
60 parts of phenyltrichlorosilane (P1);
110 parts of diphenyldichlorosilane (P2);
220 parts of methylvinyldichlorosilane.
Fully mixing the organic silicon monomers according to a certain proportion, adding the mixture into 800 parts of benzene, adding 1800 parts of butyl ether and 900 parts of water, controlling the hydrolysis temperature at 10 ℃, completing hydrolysis within 4 hours, performing water washing and water washing separation after the hydrolysis is completed, then adding 0.8 part of platinum chloride catalyst, adding 180 parts of regulator hydroxyl organic silicon low molecule, reducing the gel degree, then adding toluene, and regulating the solid content to be 50% solution, thus obtaining the organic silicon resin.
Neutralizing the discharged waste acid water after hydrolysis, water washing and water washing separation by a neutralizer added with active alkaline substances, and filtering and discharging salt-containing wastewater by a filter after the neutralization of the hydrolyzed waste acid water; neutralizing the waste acid water discharged by washing with water by using a neutralizer, separating by using a separator, and discharging salt-containing waste water; the waste acid water after washing and separation is neutralized by a neutralizer, and then secondary circulating water separated by a separator is returned to the hydrolysis and washing processes for recycling.
One ton of resin was produced and the discharge of the brine waste after neutralization after separation was only 4 tons.
Example 3
The raw materials for synthesizing the organic silicon resin comprise the following components in percentage by mass:
120 parts of methyltrichlorosilane (M1);
60 parts of dimethyldichlorosilane (M2);
60 parts of phenyltrichlorosilane (P1);
110 parts of diphenyldichlorosilane (P2);
140 parts of epoxy-containing organosilicon coupling agent.
Fully mixing the organic silicon monomers according to a certain proportion, adding the mixture into 500 parts of benzene, adding 1800 parts of butanone and 1000 parts of water, controlling the hydrolysis temperature at 10 ℃, completing hydrolysis within 4 hours, performing water washing and water washing separation after the hydrolysis is completed, then adding 1 part of zinc acetate catalyst, adding 140 parts of regulator hydroxyl organic silicon low molecule, reducing the degree of gelation, then adding toluene, and adjusting the solid content to be 50% solution, thus obtaining the organic silicon resin.
Neutralizing the discharged waste acid water after hydrolysis, water washing and water washing separation by a neutralizer added with active alkaline substances, and filtering and discharging salt-containing wastewater by a filter after the neutralization of the hydrolyzed waste acid water; neutralizing the waste acid water discharged by washing with water by using a neutralizer, separating by using a separator, and discharging salt-containing waste water; the waste acid water after washing and separation is neutralized by a neutralizer, and then secondary circulating water separated by a separator is returned to the hydrolysis and washing processes for recycling.
One ton of resin was produced and the discharge of the brine waste after neutralization after separation was only 4 tons.
Comparative example 1
The raw materials for synthesizing the organic silicon resin comprise the following components in percentage by mass:
120 parts of methyltrichlorosilane (M1);
80 parts of dimethyldichlorosilane (M2);
80 parts of phenyltrichlorosilane (P1);
120 parts of diphenyldichlorosilane (P2);
120 parts of ester-containing organosilicon coupling agent.
Fully mixing the organic silicon monomers in proportion, adding the mixture into 600 parts of benzene, adding 1200 parts of butanone and 600 parts of water, controlling the hydrolysis temperature at 5 ℃, completing hydrolysis within 5 hours, performing water washing and water washing separation after the hydrolysis is completed, then adding 1 part of lead naphthenate catalyst, adding 140 parts of epoxy group organic silicon low molecule serving as an adjusting agent, reducing the degree of gelation, then adding toluene, and adjusting the solid content to be 50% solution to obtain the organic silicon resin.
One ton of resin was produced and the discharge of the salt-containing wastewater after the neutralization was 10 tons after the separation.

Claims (8)

1. The method for preparing the organic silicon resin with energy conservation and emission reduction is characterized by comprising the following steps:
(1) preparing raw materials according to a proportion;
the raw materials comprise basic organic silicon monomers, special organic silicon monomers and organic solvents;
(2) hydrolysis: fully mixing the organosilicon monomers in the step (1) in proportion, and adding the mixture into an organic solvent for co-hydrolysis; feeding the waste acid water generated by hydrolysis into a neutralizer added with active alkaline substances for neutralization, and filtering and discharging salt-containing wastewater through a filter;
(3) after hydrolysis, washing with water, separating by washing with water, then adding a catalyst for telomerization and polycondensation, adding a regulator to reduce the degree of gelation, and regulating the mass fraction of the silicone resin solution to 50% to obtain the silicone resin;
feeding the waste acid water discharged by washing into a neutralizer added with active alkaline substances for neutralization, separating by a separator, and discharging salt-containing wastewater; the waste acid water after washing and separation is sent into a neutralizer added with active alkaline substances for neutralization, and secondary circulating water separated by the separator is returned to the hydrolysis and washing processes for recycling.
2. The method for preparing the organic silicon resin with the functions of energy conservation and emission reduction as claimed in claim 1, wherein the basic organic silicon monomer in the step (1) is: monomethyltrichlorosilane (M1), dimethyldichlorosilane (M2), monophenyltrichlorosilane (P1), diphenyldichlorosilane (P2); the special organic silicon monomer is as follows: one or more organosilicon monomer materials of organosilicon monomer containing double bond group, organosilicon monomer containing active hydrogen and silane coupling agent; the organic solvent is: cyclohexanone, butanone, ethyl acetate or butyl ethyl ether.
3. The method for preparing organic silicon resin with energy conservation and emission reduction as claimed in claim 2, wherein the organic silicon monomer containing double bond groups is methyl vinyl dichlorosilane, the organic silicon monomer containing active hydrogen is methyl hydrogen dichlorosilane, the silane coupling agent is epoxy-containing triethoxysilane, ester-containing triethoxysilane, and amino-containing triethoxysilane and acryloyl-containing triethoxysilane.
4. The method for preparing the organic silicon resin with the functions of energy conservation and emission reduction as claimed in claim 1, wherein in the total organic silicon monomer, the ratio of the number of organic groups R on silicon atoms to the number of silicon atoms, R/Si is 1.0-1.6, the number of phenyl groups accounts for 15-60% of the total number of R, and the mass of the special organic silicon monomer accounts for 10-40% of the total mass of the organic silicon monomer; the dosage of the organic solvent is 2-4 times of the mass of the water; the water amount is 1-2 times of the total mass of the organic silicon monomer.
5. The method for preparing the organic silicon resin with the effects of energy conservation and emission reduction as claimed in claim 1, wherein the active alkaline substance is strong alkali inorganic base, Lewis base, hydroxylamine or strong alkali ion exchange resin.
6. The method for preparing the organic silicon resin with the functions of energy conservation and emission reduction as claimed in claim 1, wherein the cohydrolysis temperature is 4-10 ℃.
7. The method for preparing the organic silicon resin with the effects of energy conservation and emission reduction as claimed in claim 1, wherein the added catalyst is a transition metal salt catalyst, and the dosage of the transition metal salt catalyst is 1-2 per mill of the total mass of the organic silicon monomer.
8. The method for preparing the organic silicon resin with the functions of energy conservation and emission reduction as claimed in claim 1, wherein the added catalyst is platinum chloride, cobalt naphthenate, lead acetate or zinc acetate; the added regulator is organosilicon oligomer with hydroxyl, epoxy or ester group, and the dosage of the organosilicon oligomer is 20-30% of the total mass of the organosilicon monomer.
CN201911021987.4A 2019-10-25 2019-10-25 Method for preparing organic silicon resin with energy conservation and emission reduction Pending CN110835410A (en)

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