CN113185471A - Trihydroxyethyl isocyanurate decoloring method and decoloring agent - Google Patents
Trihydroxyethyl isocyanurate decoloring method and decoloring agent Download PDFInfo
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- CN113185471A CN113185471A CN202110394091.1A CN202110394091A CN113185471A CN 113185471 A CN113185471 A CN 113185471A CN 202110394091 A CN202110394091 A CN 202110394091A CN 113185471 A CN113185471 A CN 113185471A
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- catalyst
- reaction
- decoloring
- agent
- organic solvent
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/30—Only oxygen atoms
- C07D251/34—Cyanuric or isocyanuric esters
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A trihydroxyethyl isocyanuric ester decolouring method and decolouring agent, in the field of chemical synthesis technology, cyanuric acid and ethylene oxide carry on the addition reaction in organic solvent under the catalysis of catalyst, decolour the reaction solution after the reaction is finished and filter, cool and crystallize and get the purpose thing; the organic solvent is DMF, the catalyst is a solid-liquid mixed catalyst containing tetramethylammonium chloride and triethylamine, and the decolorizing agent is diatomite. The invention greatly improves the quality of the product, shortens the production period and improves the yield of the product.
Description
Technical Field
The invention relates to a method for decoloring trihydroxyethyl isocyanurate and a decoloring agent, belonging to the technical field of chemical synthesis.
Background
The prior art of trihydroxyethyl isocyanurate is that cyanuric acid and ethylene oxide are subjected to addition reaction in an organic solvent of ethylene glycol monomethyl ether under the catalysis of a catalyst of benzyltriethylammonium chloride, the addition reaction is generally carried out, then a concentrated solvent is used indiscriminately, a refined solvent is added for dissolution, activated carbon is added for decolorization, then the temperature is reduced, a wet finished product is obtained by centrifugation, the solvent is recovered from mother liquor for next refining, and the process can obtain a pure product by recrystallization of the concentrated solvent. Long process and high energy consumption.
Disclosure of Invention
The invention provides a method for decoloring trihydroxyethyl isocyanurate and a decoloring agent, wherein a proper solvent is selected to replace the original ethylene glycol monomethyl ether, so that the trihydroxyethyl isocyanurate can be used as a reaction solvent and also can be used as a refined solvent.
The purpose of the invention is realized by the following technical scheme:
a trihydroxyethyl isocyanuric ester decolouring method and decolouring agent, cyanuric acid and ethylene oxide carry on the addition reaction in organic solvent under the catalysis of catalyst, decolour the reaction solution after the reaction is finished and filter, cool and crystallize and get the purpose thing; the organic solvent is DMF, the catalyst is a solid-liquid mixed catalyst containing tetramethylammonium chloride and triethylamine, and the decolorizing agent is diatomite.
The catalyst is preferably a solid-liquid mixed catalyst consisting of tetramethylammonium chloride and triethylamine.
More preferably, the weight ratio of the tetramethylammonium chloride to the triethylamine is 1-4: 1.
The dosage of the tetramethylammonium chloride is 1.5 to 3 percent of the weight of the cyanuric acid.
The weight ratio of cyanuric acid to ethylene oxide is 1: 1 to 1.3.
The dosage of the organic solvent is 1.5-3 times of the weight of cyanuric acid.
The reaction temperature of the addition reaction is 90-100 ℃.
The reaction pressure of the addition reaction is 5-6 kg.
The invention adopts alcohol methanol and ethanol with low boiling point as reaction solvents. Due to the change of the reaction solvent, the original catalyst triethylbenzylammonium chloride is not suitable for the addition reaction of a new solvent system, and the new solvent has stronger polarity than the original solvent, so the pH of the reaction system is acidic, and a phase transfer catalyst with strong alkalinity needs to be screened for carrying out the catalytic reaction. The inventor researches and discovers that: the most rational catalyst varieties and the dosage are as follows, the solid catalyst tetramethylammonium chloride and the liquid catalyst triethylamine are used together, the effect is best, and the indexes of reaction time, product quality, yield and the like can be simultaneously met. The dosage of the solid catalyst is 1.5-3% of the weight ratio of the raw material cyanuric acid, and the weight ratio of the solid catalyst to the liquid catalyst is 1-4: 1. The most preferred amount of liquid catalyst is 50% by weight of the solid catalyst.
The invention has the beneficial effects that:
by adopting the technical scheme of the invention, the comprehensive yield of the product can be improved to 95% from 88% in the prior art, the product quality is greatly improved, the production period is shortened, the product yield is improved, the application times of leftovers are improved to 80 times from 30 times, the raw material consumption is effectively reduced, the reaction time is shortened, the product quality is further ensured, and the guarantee is provided for producing the high-quality trihydroxyethyl isocyanurate.
Detailed Description
The detailed process of the most preferred technical scheme is as follows: adding cyanuric acid, DMF, tetramethylammonium chloride and triethylamine into a pressure reaction kettle, introducing ethylene oxide into the pressure reaction kettle within 2-3 hours at 90-100 ℃ under the pressure of 5-6 kilograms, then preserving heat for 1-2 hours, cooling to 25-35 ℃, adding activated carbon, preserving heat for decoloring at 50-60 ℃, removing an activated carbon layer through heat filtration, cooling filtrate to 10-15 ℃, centrifuging to obtain a wet finished product, and drying to obtain a finished product. The weight ratio of the tetramethylammonium chloride to the triethylamine is 1-4: 1, the amount of the tetramethylammonium chloride is 1.5-3% of the weight of the cyanuric acid, and the weight ratio of the cyanuric acid to the ethylene oxide is 1: 1-1.3, and the dosage of the organic solvent is 1.5-3 times of the weight of cyanuric acid.
Claims (1)
1. A trihydroxyethyl isocyanuric ester decolouring method and decolouring agent, cyanuric acid and ethylene oxide carry on the addition reaction in organic solvent under the catalysis of catalyst, decolour the reaction solution after the reaction is finished and filter, cool and crystallize and get the purpose thing; the organic solvent is DMF, the catalyst is a solid-liquid mixed catalyst containing tetramethylammonium chloride and triethylamine, and the decolorizing agent is diatomite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110394091.1A CN113185471A (en) | 2021-04-13 | 2021-04-13 | Trihydroxyethyl isocyanurate decoloring method and decoloring agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110394091.1A CN113185471A (en) | 2021-04-13 | 2021-04-13 | Trihydroxyethyl isocyanurate decoloring method and decoloring agent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113185471A true CN113185471A (en) | 2021-07-30 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110394091.1A Pending CN113185471A (en) | 2021-04-13 | 2021-04-13 | Trihydroxyethyl isocyanurate decoloring method and decoloring agent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113185471A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1170044A (en) * | 1968-02-29 | 1969-11-12 | Allied Chem | Improved process for the production of tris-(2-hydroxyalkyl) isocyamurates |
| US5719281A (en) * | 1995-03-22 | 1998-02-17 | Basf Aktiengesellschaft | Preparation of 1/3/5-Tris(2-Hydroxyalkyl) isocyanurates |
| CN1923821A (en) * | 2006-09-28 | 2007-03-07 | 宜兴市中正化工有限公司 | Synthesis method of trihydroxyethyl isocyanuric ester |
| CN104710375A (en) * | 2015-02-27 | 2015-06-17 | 宜兴市中正化工有限公司 | Method for producing THEIC |
-
2021
- 2021-04-13 CN CN202110394091.1A patent/CN113185471A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1170044A (en) * | 1968-02-29 | 1969-11-12 | Allied Chem | Improved process for the production of tris-(2-hydroxyalkyl) isocyamurates |
| US5719281A (en) * | 1995-03-22 | 1998-02-17 | Basf Aktiengesellschaft | Preparation of 1/3/5-Tris(2-Hydroxyalkyl) isocyanurates |
| CN1923821A (en) * | 2006-09-28 | 2007-03-07 | 宜兴市中正化工有限公司 | Synthesis method of trihydroxyethyl isocyanuric ester |
| CN104710375A (en) * | 2015-02-27 | 2015-06-17 | 宜兴市中正化工有限公司 | Method for producing THEIC |
Non-Patent Citations (1)
| Title |
|---|
| 吕海金: "化工专业导论", vol. 1, 中国海洋大学出版社, pages: 78 * |
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Address after: 272200 Jining Chemical Industrial Development Zone, Hu Ji Town, Jinxiang County, Jining, Shandong Applicant after: Shandong Jianbang New Material Co.,Ltd. Address before: 272200 Jining Chemical Industrial Development Zone, Hu Ji Town, Jinxiang County, Jining, Shandong Applicant before: JINING JIANBANG CHEMICAL CO.,LTD. |
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