CN110272394A - A kind of preparation method of s-triazine - Google Patents
A kind of preparation method of s-triazine Download PDFInfo
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- CN110272394A CN110272394A CN201910628073.8A CN201910628073A CN110272394A CN 110272394 A CN110272394 A CN 110272394A CN 201910628073 A CN201910628073 A CN 201910628073A CN 110272394 A CN110272394 A CN 110272394A
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- triazine
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/60—Preparation of compounds having groups or groups
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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
- C07D251/14—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 hydrogen or carbon atoms directly attached to at least one ring carbon atom
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention provides a kind of preparation method of s-triazine, is related to a kind of technical field of chemical synthesis.The invention reacts it with s-triazine generation, so that s-triazine ingredient becomes 0.05% from 0.3-0.5%, greatly improves the product quality of trimethyl orthoformate by adjusting technical process by being passed through excessive hydrogen chloride.
Description
Technical field
The present invention relates to a kind of technical field of chemical synthesis, more particularly to a kind of preparation method of s-triazine.
Background technique
Trimethyl orthoformate (trimethyl orthoformate), also known as trimethoxy-methane (HC (OCH3) 3) are weights
The organic synthesis intermediate wanted.Medical aspect is for synthesizing vitamin A, vitamin B1, sulfanilamide (SN), antibiotic etc.；It is used in terms of coating
In the dehydration of polyurethane or epoxy coating to prevent from hardening；Also it is used for perfume synthesis, market dosage to increase year by year.
Summary of the invention
Aiming at the shortcomings existing in the above problems, the present invention provides a kind of preparation method of s-triazine, makes its adjustment
Technical process reacts it with s-triazine generation, so that s-triazine ingredient is by 0.3-0.5% by being passed through excessive hydrogen chloride
Become 0.05%, greatly improves the product quality of trimethyl orthoformate.
To solve the above-mentioned problems, the present invention provides a kind of preparation method of s-triazine, wherein the following steps are included:
S10, start to lead to when at extremely -5~+5 DEG C of salt oven temperature drop at addition solvent o-dichlorohenzene and methanol in salt oven
Gas process kettle temperature is controlled at 0 DEG C or less；
S20, it after having led to gas, flows plus hydrogen cyanide, 6~14h is added, stream plus hydrogen cyanide temperature control≤5 DEG C carry out salt-forming reaction；
S30, end of reaction at saline solution regardless of exsolution agent, be directly transferred to alcoholysis kettle carry out subsequent processing operation, at saline solution
Vacuum removal under stiring；
S40, methanol solution is added, obtains alcoholysis reaction liquid within insulation reaction 4~5 hours at 40 DEG C~60 DEG C；
S50, the step of refining include being centrifugated to alcoholysis reaction liquid, obtain trimethyl orthoformate crude product；
S60, hydrogen chloride is passed through into trimethyl orthoformate crude product, hydrogen chloride is reacted with s-triazine, forms hydrochloride；
S70, hydrochloride is crystallized, is static, after sedimentation, s-triazine ingredient is become from 0.3-0.5% in supernatant
0.05%.
Preferably, in the step S20, adding hydrogen cyanide and keeping the temperature -5~+5 DEG C again and react 2~3 hours terminates.
Preferably, in the step S30, vacuum degree -0.07~-0.09Mpa removes 2~4 at 0~10 DEG C of temperature
Hour.
Compared with prior art, the invention has the following advantages that
The present invention is by adjusting technical process, by being passed through excessive hydrogen chloride, reacts it with s-triazine generation, so that
S-triazine ingredient becomes 0.05% from 0.3-0.5%, greatly improves the product quality of trimethyl orthoformate.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, the present invention is made below with reference to example
It is further described, but example is not as a limitation of the invention.
The embodiment of the present invention
A kind of preparation method of s-triazine, comprising the following steps:
S10, start to lead to when at extremely -5~+5 DEG C of salt oven temperature drop at addition solvent o-dichlorohenzene and methanol in salt oven
Gas process kettle temperature is controlled at 0 DEG C or less；
S20, it after having led to gas, flows plus hydrogen cyanide, 6~14h is added, stream plus hydrogen cyanide temperature control≤5 DEG C carry out salt-forming reaction；
Adding hydrogen cyanide and keeping the temperature -5~+5 DEG C again and react 2~3 hours terminates；
S30, end of reaction at saline solution regardless of exsolution agent, be directly transferred to alcoholysis kettle carry out subsequent processing operation, at saline solution
Vacuum removal under stiring；Vacuum degree -0.07~-0.09Mpa removes 2~4 hours at 0~10 DEG C of temperature；
S40, methanol solution is added, obtains alcoholysis reaction liquid within insulation reaction 4~5 hours at 40 DEG C~60 DEG C；
S50, the step of refining include being centrifugated to alcoholysis reaction liquid, obtain trimethyl orthoformate crude product；
S60, hydrogen chloride is passed through into trimethyl orthoformate crude product, hydrogen chloride is reacted with s-triazine, forms hydrochloride；
S70, hydrochloride is crystallized, is static, after sedimentation, s-triazine ingredient is become from 0.3-0.5% in supernatant
0.05%.
In the present embodiment, hydrogen chloride is passed through into trimethyl orthoformate crude product, hydrogen chloride is reacted with s-triazine, forms hydrochloric acid
Salt, after crystallization, static, sedimentation, s-triazine ingredient becomes 0.05% from 0.3-0.5% in supernatant, improves product quality.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (3)
1. a kind of preparation method of s-triazine, which comprises the following steps:
S10, at solvent o-dichlorohenzene and methanol are added in salt oven, when at salt oven temperature drop to -5~+5 DEG C, start to ventilate into
Journey kettle temperature is controlled at 0 DEG C or less；
S20, it after having led to gas, flows plus hydrogen cyanide, 6~14h is added, stream plus hydrogen cyanide temperature control≤5 DEG C carry out salt-forming reaction；
S30, end of reaction at saline solution regardless of exsolution agent, be directly transferred to alcoholysis kettle carry out subsequent processing operation, stirred at saline solution
Mix lower vacuum removal；
S40, methanol solution is added, obtains alcoholysis reaction liquid within insulation reaction 4~5 hours at 40 DEG C~60 DEG C；
S50, the step of refining include being centrifugated to alcoholysis reaction liquid, obtain trimethyl orthoformate crude product；
S60, hydrogen chloride is passed through into trimethyl orthoformate crude product, hydrogen chloride is reacted with s-triazine, forms hydrochloride；
S70, hydrochloride is crystallized, is static, after sedimentation, s-triazine ingredient becomes 0.05% from 0.3-0.5% in supernatant.
2. the preparation method of s-triazine as described in claim 1, which is characterized in that in the step S20, add hydrogen cyanide
Keep the temperature -5~+5 DEG C of reactions again terminates for 2~3 hours.
3. the preparation method of s-triazine as described in claim 1, which is characterized in that in the step S30, vacuum degree-
0.07~-0.09Mpa is removed 2~4 hours at 0~10 DEG C of temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910628073.8A CN110272394A (en) | 2019-07-12 | 2019-07-12 | A kind of preparation method of s-triazine |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910628073.8A CN110272394A (en) | 2019-07-12 | 2019-07-12 | A kind of preparation method of s-triazine |
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| CN110272394A true CN110272394A (en) | 2019-09-24 |
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| CN201910628073.8A Pending CN110272394A (en) | 2019-07-12 | 2019-07-12 | A kind of preparation method of s-triazine |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1657516A (en) * | 2004-02-20 | 2005-08-24 | 顾利华 | Process for preparing high-purity orthoformate |
| CN102367221A (en) * | 2011-09-01 | 2012-03-07 | 重庆紫光化工股份有限公司 | Preparation method of ortho-formate |
| CN103130622A (en) * | 2011-11-28 | 2013-06-05 | 重庆紫光化工股份有限公司 | Preparation method of trimethyl orthoformate |
| CN103483165A (en) * | 2013-09-25 | 2014-01-01 | 河北诚信有限责任公司 | Green process for preparing orthoformate |
| CN103739463A (en) * | 2014-01-02 | 2014-04-23 | 淄博万昌科技股份有限公司 | Simple and convenient method for producing high-purity ortho-formate |
| CN106946666A (en) * | 2017-03-21 | 2017-07-14 | 临沭县华盛化工有限公司 | The synthesis technique of trimethyl orthoformate |
-
2019
- 2019-07-12 CN CN201910628073.8A patent/CN110272394A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1657516A (en) * | 2004-02-20 | 2005-08-24 | 顾利华 | Process for preparing high-purity orthoformate |
| CN102367221A (en) * | 2011-09-01 | 2012-03-07 | 重庆紫光化工股份有限公司 | Preparation method of ortho-formate |
| CN103130622A (en) * | 2011-11-28 | 2013-06-05 | 重庆紫光化工股份有限公司 | Preparation method of trimethyl orthoformate |
| CN103483165A (en) * | 2013-09-25 | 2014-01-01 | 河北诚信有限责任公司 | Green process for preparing orthoformate |
| CN103739463A (en) * | 2014-01-02 | 2014-04-23 | 淄博万昌科技股份有限公司 | Simple and convenient method for producing high-purity ortho-formate |
| CN106946666A (en) * | 2017-03-21 | 2017-07-14 | 临沭县华盛化工有限公司 | The synthesis technique of trimethyl orthoformate |
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Application publication date: 20190924 |