CN114213610A - Powder phenolic resin and production process thereof - Google Patents
Powder phenolic resin and production process thereof Download PDFInfo
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- CN114213610A CN114213610A CN202210034498.8A CN202210034498A CN114213610A CN 114213610 A CN114213610 A CN 114213610A CN 202210034498 A CN202210034498 A CN 202210034498A CN 114213610 A CN114213610 A CN 114213610A
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- phenolic resin
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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
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/10—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with phenol
Abstract
The invention discloses a powder phenolic resin, which comprises phenol, formaldehyde and an acid catalyst, and a production process of the powder phenolic resin comprises the following steps: (1) synthesizing: putting phenol and formaldehyde in a certain molar ratio into a production container, then adding a catalyst hydrochloric acid into the container, heating the production container to a certain temperature after adding the hydrochloric acid, stopping heating, heating the materials in the production container continuously after the materials generate heat through a polycondensation reaction, and then dehydrating the materials to form solid phenolic resin; (2) crushing; (3) resin extraction; (4) secondary condensation; (5) neutralizing and precipitating. The proportion of raw materials added in the production of the phenolic resin is increased, so that the time required by the production process is shortened, the resin in the wastewater is recovered after the production is finished, the production cost is reduced, and meanwhile, the formaldehyde and the phenol in the wastewater are removed, so that the damage of the wastewater to the surrounding environment is avoided.
Description
Technical Field
The invention relates to the technical field of phenolic resin, in particular to powder phenolic resin and a production process thereof.
Background
Phenolic resin, also called bakelite, is colorless or yellowish brown transparent, and is usually sold in the market with a colorant in red, yellow, black, green, brown, blue and other colors, in the form of granules or powder. The corrosion inhibitor is resistant to weak acid and weak base, can be decomposed when meeting strong acid, and can be corroded when meeting strong base. Insoluble in water, and soluble in organic solvents such as acetone and alcohol. Obtained by condensation polymerization of phenol formaldehyde or derivatives thereof. The solid phenolic resin is yellow, transparent and amorphous massive substance, is reddish due to containing free phenol, has an average specific gravity of about 1.7, is easily soluble in alcohol, is insoluble in water, and is stable to water, weak acid and weak base solution. The resin is prepared by condensation polymerization of phenol and formaldehyde under the condition of catalyst, neutralization and water washing. The catalyst can be divided into two types of thermosetting and thermoplastic. The phenolic resin has good acid resistance, mechanical property and heat resistance, and can be widely applied to industries of corrosion prevention engineering, adhesives, flame retardant materials, grinding wheel manufacturing and the like
At present, a large amount of industrial wastewater is generated in the production of phenolic resin in the market, most of the wastewater is directly discharged after primary purification, and great damage is caused to the surrounding environment, so that a powder phenolic resin and a production process thereof are provided, so as to solve the problems.
Disclosure of Invention
The invention aims to provide a powder-particle phenolic resin and a production process thereof, which aim to solve the problems that a large amount of industrial wastewater is generated in the production of phenolic resin in the market at present, most of the wastewater is directly discharged after primary purification, and the surrounding environment is greatly damaged.
In order to achieve the purpose, the invention provides the following technical scheme: a phenolic resin in powder form comprising said phenol, formaldehyde and an acidic catalyst.
Preferably, the content of phenol used in the preparation process is required to be 96%, the content of formaldehyde used in the preparation process is required to be more than 34%, the content of precipitate is less than 1%, and hydrochloric acid is selected as the acid catalyst.
Preferably, the production process of the powder-particle phenolic resin comprises the following steps:
(1) synthesizing: putting phenol and formaldehyde in a certain molar ratio into a production container, then adding a catalyst hydrochloric acid into the container, heating the production container to a certain temperature after adding the hydrochloric acid, stopping heating, heating the materials in the production container continuously after the materials generate heat through a polycondensation reaction, and then dehydrating the materials to form solid phenolic resin;
(2) crushing: putting the solid phenolic resin generated in the step (1) into a crushing device for crushing, and sieving the crushed phenolic resin;
(3) resin extraction: waste water generated in the production process is pumped into a primary condensation kettle for delayed condensation, so that residual resin in the waste water is recycled;
(4) secondary condensation: adding a medicament capable of taking out formaldehyde and phenol into the wastewater for condensation treatment;
(5) neutralizing and precipitating: mixing the wastewater after secondary condensation with the pump flushing wastewater, and adding lime milk to adjust the pH value.
Preferably, in the step (1), the molar ratio of phenol to formaldehyde is 7:6, the mass ratio of the acid catalyst hydrochloric acid is 0.1-0.3%, the production container is initially heated to 80-90 ℃, and the temperature of the reaction container is raised to 95-100 ℃ by secondary heat release.
Preferably, the reaction time of the delayed condensation reaction in the step (3) is 5h to 10h, the reaction temperature is 90 ℃ to 110 ℃, and the condensation reaction temperature in the step (4) is 95 ℃ to 100 ℃.
Preferably, after the lime milk is added in the step (5), the pH value is adjusted to 7-8, the mixture is kept standing for 2-4 h, and the mixing ratio of the acidic wastewater after secondary condensation and the pump flushing wastewater is 10: 6.
Compared with the prior art, the invention has the beneficial effects that: the proportion of raw materials added in the production of the phenolic resin is increased, so that the time required by the production process is shortened, the resin in the wastewater is recovered after the production is finished, the production cost is reduced, and meanwhile, the formaldehyde and the phenol in the wastewater are removed, so that the damage of the wastewater to the surrounding environment is avoided.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
A phenolic resin in powder form comprising said phenol, formaldehyde and an acidic catalyst.
The content of phenol used in the preparation process is required to be 94%, the content of formaldehyde used in the preparation process is required to be more than 30%, the content of precipitate is less than 2%, and hydrochloric acid is selected as the acid catalyst.
A production process of powder phenolic resin comprises the following steps:
(1) synthesizing: putting phenol and formaldehyde with a certain molar ratio into a production container, then adding a catalyst hydrochloric acid into the container, heating the production container to a certain temperature after adding the hydrochloric acid, stopping heating, heating the materials in the production container continuously after the materials are subjected to polycondensation reaction, dehydrating the materials to form solid phenolic resin, primarily heating the production container to 60 ℃, and heating the reaction container to 75 ℃ after secondary heat release, wherein the molar ratio of the phenol to the formaldehyde is 10:8, the mass ratio of the acid catalyst hydrochloric acid is 0.5%;
(2) crushing: putting the solid phenolic resin generated in the step (1) into a crushing device for crushing, and sieving the crushed phenolic resin;
(3) resin extraction: waste water generated in the production process is injected into a primary condensation kettle for delayed condensation, so that residual resin in the waste water is recovered, the reaction time of the delayed condensation reaction is 3 hours, and the reaction temperature is 80 ℃;
(4) secondary condensation: adding a medicament capable of taking out formaldehyde and phenol into the wastewater for condensation treatment, wherein the condensation reaction temperature in the step (4) is 80 ℃;
(5) neutralizing and precipitating: mixing the wastewater after the secondary condensation with the pump flushing wastewater, then adding lime milk to adjust the pH value, adding the lime milk to adjust the pH value to 9, and continuously standing for 5h, wherein the mixing ratio of the acidic wastewater after the secondary condensation to the pump flushing wastewater is 10: 4.
Example two
A phenolic resin in powder form comprising said phenol, formaldehyde and an acidic catalyst.
The content of phenol used in the preparation process is required to be 96%, the content of formaldehyde used in the preparation process is required to be more than 40%, the content of precipitate is less than 0.5%, and hydrochloric acid is selected as the acid catalyst.
A production process of powder phenolic resin comprises the following steps:
(1) synthesizing: putting phenol and formaldehyde with a certain molar ratio into a production container, then adding a catalyst hydrochloric acid into the container, heating the production container to a certain temperature after adding the hydrochloric acid, stopping heating, heating materials in the production container continuously after the materials generate heat through a polycondensation reaction, dehydrating the materials to form solid phenolic resin, heating the production container to 90 ℃ primarily, and heating the reaction container to 95 ℃ through secondary heat release;
(2) crushing: putting the solid phenolic resin generated in the step (1) into a crushing device for crushing, and sieving the crushed phenolic resin;
(3) resin extraction: waste water generated in the production process is injected into a primary condensation kettle for delayed condensation, so that residual resin in the waste water is recovered, the reaction time of the delayed condensation reaction is 4 hours, and the reaction temperature is 120 ℃;
(4) secondary condensation: adding a medicament capable of taking out formaldehyde and phenol into the wastewater for condensation treatment, wherein the condensation reaction temperature in the step (4) is 95 ℃;
(5) neutralizing and precipitating: mixing the wastewater after the secondary condensation with the pump flushing wastewater, then adding lime milk to adjust the pH value, adding the lime milk to adjust the pH value to 6, and continuously standing for 3h, wherein the mixing ratio of the acidic wastewater after the secondary condensation to the pump flushing wastewater is 6: 10.
EXAMPLE III
A phenolic resin in powder form comprising said phenol, formaldehyde and an acidic catalyst.
The content of phenol used in the preparation process is required to be 96%, the content of formaldehyde used in the preparation process is required to be more than 34%, the content of precipitate is less than 1%, and hydrochloric acid is selected as the acid catalyst.
A production process of powder phenolic resin comprises the following steps:
(1) synthesizing: putting phenol and formaldehyde with a certain molar ratio into a production container, then adding a catalyst hydrochloric acid into the container, heating the production container to a certain temperature after adding the hydrochloric acid, stopping heating, heating the materials in the production container continuously after the materials are subjected to polycondensation reaction, dehydrating the materials to form solid phenolic resin, heating the production container to 40 ℃ primarily, and heating the reaction container to 60 ℃ after secondary heat release, wherein the molar ratio of the phenol to the formaldehyde is 4:7, the mass ratio of the acid catalyst hydrochloric acid is 0.1%;
(2) crushing: putting the solid phenolic resin generated in the step (1) into a crushing device for crushing, and sieving the crushed phenolic resin;
(3) resin extraction: waste water generated in the production process is injected into a primary condensation kettle for delayed condensation, so that residual resin in the waste water is recovered, the reaction time of the delayed condensation reaction is 3 hours, and the reaction temperature is 70 ℃;
(4) secondary condensation: adding a medicament capable of taking out formaldehyde and phenol into the wastewater for condensation treatment, wherein the condensation reaction temperature in the step (4) is 105 ℃;
(5) neutralizing and precipitating: mixing the wastewater after the secondary condensation with the pump flushing wastewater, then adding lime milk to adjust the pH value, adding the lime milk to adjust the pH value to 8, and continuously standing for 3.5h, wherein the mixing ratio of the acidic wastewater after the secondary condensation to the pump flushing wastewater is 12: 8.
Example four
A phenolic resin in powder form comprising said phenol, formaldehyde and an acidic catalyst.
The content of phenol used in the preparation process is required to be 96%, the content of formaldehyde used in the preparation process is required to be more than 40%, the content of precipitate is less than 1.5%, and hydrochloric acid is selected as the acid catalyst.
A production process of powder phenolic resin comprises the following steps:
(1) synthesizing: putting phenol and formaldehyde with a certain molar ratio into a production container, then adding a catalyst hydrochloric acid into the container, heating the production container to a certain temperature after adding the hydrochloric acid, stopping heating, heating the materials in the production container continuously after the materials generate heat through a polycondensation reaction, dehydrating the materials to form solid phenolic resin, heating the production container to 90 ℃ primarily, and heating the reaction container to 95 ℃ through secondary heat release;
(2) crushing: putting the solid phenolic resin generated in the step (1) into a crushing device for crushing, and sieving the crushed phenolic resin;
(3) resin extraction: waste water generated in the production process is injected into a primary condensation kettle for delayed condensation, so that residual resin in the waste water is recovered, the reaction time of the delayed condensation reaction is 5 hours, and the reaction temperature is 90 ℃;
(4) secondary condensation: adding a medicament capable of taking out formaldehyde and phenol into the wastewater for condensation treatment, wherein the condensation reaction temperature in the step (4) is 95 ℃;
(5) neutralizing and precipitating: mixing the wastewater after the secondary condensation with the pump flushing wastewater, then adding lime milk to adjust the pH value, adding the lime milk to adjust the pH value to 7-8, and continuously standing for 2h, wherein the mixing ratio of the acidic wastewater after the secondary condensation to the pump flushing wastewater is 8: 12.
EXAMPLE five
A phenolic resin in powder form comprising said phenol, formaldehyde and an acidic catalyst.
The content of phenol used in the preparation process is required to be 96%, the content of formaldehyde used in the preparation process is required to be more than 34%, the content of precipitate is less than 1%, and hydrochloric acid is selected as the acid catalyst.
A production process of powder phenolic resin comprises the following steps:
(1) synthesizing: putting phenol and formaldehyde with a certain molar ratio into a production container, then adding a catalyst hydrochloric acid into the container, heating the production container to a certain temperature after adding the hydrochloric acid, stopping heating, heating materials in the production container continuously after the materials generate heat through a polycondensation reaction, dehydrating the materials to form solid phenolic resin, wherein the molar ratio of the phenol to the formaldehyde is 7:6, the mass ratio of the acid catalyst hydrochloric acid is 0.1-0.3%, primarily heating the production container to 80-90 ℃, and heating the reaction container to 95-100 ℃ through secondary heat release;
(2) crushing: putting the solid phenolic resin generated in the step (1) into a crushing device for crushing, and sieving the crushed phenolic resin;
(3) resin extraction: waste water generated in the production process is injected into a primary condensation kettle for delayed condensation, so that residual resin in the waste water is recovered, the reaction time of the delayed condensation reaction is 5-10 h, and the reaction temperature is 90-110 ℃;
(4) secondary condensation: adding a medicament capable of taking out formaldehyde and phenol into the wastewater for condensation treatment, wherein the condensation reaction temperature in the step (4) is 95-100 ℃;
(5) neutralizing and precipitating: mixing the wastewater after the secondary condensation with the pump flushing wastewater, then adding lime milk to adjust the pH value, adding the lime milk to adjust the pH value to 7-8, continuously standing for 2-4 h, wherein the mixing ratio of the acidic wastewater after the secondary condensation to the pump flushing wastewater is 10: 6.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (6)
1. A phenol resin powder, comprising the phenol, formaldehyde and an acidic catalyst.
2. The phenolic resin powder and the production process thereof as claimed in claim 1, wherein: the content of phenol used in the preparation process is required to be 96%, the content of formaldehyde used in the preparation process is required to be more than 34%, the content of precipitate is less than 1%, and hydrochloric acid is selected as the acid catalyst.
3. The production process of the powder phenolic resin is characterized by comprising the following steps:
(1) synthesizing: putting phenol and formaldehyde in a certain molar ratio into a production container, then adding a catalyst hydrochloric acid into the container, heating the production container to a certain temperature after adding the hydrochloric acid, stopping heating, heating the materials in the production container continuously after the materials generate heat through a polycondensation reaction, and then dehydrating the materials to form solid phenolic resin;
(2) crushing: putting the solid phenolic resin generated in the step (1) into a crushing device for crushing, and sieving the crushed phenolic resin;
(3) resin extraction: waste water generated in the production process is pumped into a primary condensation kettle for delayed condensation, so that residual resin in the waste water is recycled;
(4) secondary condensation: adding a medicament capable of taking out formaldehyde and phenol into the wastewater for condensation treatment;
(5) neutralizing and precipitating: mixing the wastewater after secondary condensation with the pump flushing wastewater, and adding lime milk to adjust the pH value.
4. The process according to claim 3, wherein the phenolic resin powder is prepared by the following steps: in the step (1), the molar ratio of phenol to formaldehyde is 7:6, the mass ratio of the acid catalyst hydrochloric acid is 0.1-0.3%, the production container is initially heated to 80-90 ℃, and the temperature of the reaction container is raised to 95-100 ℃ by secondary heat release.
5. The process according to claim 3, wherein the phenolic resin powder is prepared by the following steps: the reaction time of the delayed condensation reaction in the step (3) is 5-10 h, the reaction temperature is 90-110 ℃, and the condensation reaction temperature in the step (4) is 95-100 ℃.
6. The process according to claim 3, wherein the phenolic resin powder is prepared by the following steps: and (3) after adding the lime milk in the step (5), adjusting the pH value to 7-8, continuously standing for 2-4 h, wherein the mixing ratio of the acidic wastewater after secondary condensation to the pump flushing wastewater is 10: 6.
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| CN202210034498.8A CN114213610A (en) | 2022-01-13 | 2022-01-13 | Powder phenolic resin and production process thereof |
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| CN202210034498.8A CN114213610A (en) | 2022-01-13 | 2022-01-13 | Powder phenolic resin and production process thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114644742A (en) * | 2022-04-22 | 2022-06-21 | 彤程电子材料(镇江)有限公司 | Preparation process of high-uniformity phenolic resin |
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