CN103880616B - The purification process of impurity and specific equipment thereof in trimethyl orthoformate - Google Patents
The purification process of impurity and specific equipment thereof in trimethyl orthoformate Download PDFInfo
- Publication number
- CN103880616B CN103880616B CN201210556889.2A CN201210556889A CN103880616B CN 103880616 B CN103880616 B CN 103880616B CN 201210556889 A CN201210556889 A CN 201210556889A CN 103880616 B CN103880616 B CN 103880616B
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- mixed bed
- trimethyl orthoformate
- impurity
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- resin mixed
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention discloses the purification process of impurity in a kind of trimethyl orthoformate, by the crude product trimethyl orthoformate pump delivery containing impurity, first after one-level paper element filtering device filters, enter from the bottom of resin mixed bed in resin mixed bed, impurity in crude product trimethyl orthoformate carries out exchange adsorption with resin in mixed bed, then enters secondary paper element filtering device and filter; Crude product trimethyl orthoformate enters the flow control of resin mixed bed at 600-700L/h, and resin mixed bed temperature controls at 12 ~ 15 DEG C; Resin in described resin mixed bed adopts 330 weakly alkaline epoxy type anion exchange resins.The present invention adopts mixed-bed resin to process, and its foreign matter content can be dropped to less than 0.001%, even can't detect impurity by chromatogram.The invention solves prior art and there is the technical problem that dust removal rate is low, loss is many, cost is high.
Description
technical fieldthe invention belongs to trimethyl orthoformate production technical field, relate to purification process and the specific equipment thereof of impurity in a kind of trimethyl orthoformate.
background technologyat present, in trimethyl orthoformate production process, often along with the generation of impurity, foreign matter content is usually in 0.5 ~ 1%(mass percent), such impurity is in the production process of follow-up medical material medicine, can have influence on its yield, concurrent raw correlated response produces other impurity, and not easily removes.Particularly in portion downstream product uses, also can make its poisoning of catalyst, greatly reduce feed stock conversion.The purification process of impurity in prior art trimethyl orthoformate, most employing membrane separating, chemical treatment or increase the methods such as distillation tower, in the trimethyl orthoformate produced, the content of impurity has been reduced to 0.01 ~ 0.02%(mass percent), but have that loss is many, cost is high, also have influence on the use of derived product.
summary of the inventionthe object of the invention is to solve prior art and there is the technical problem that dust removal rate is low, loss is many, cost is high, the purification process of impurity in a kind of trimethyl orthoformate is provided; Another object of the present invention is to provide the specific equipment of impurity purifying in a kind of trimethyl orthoformate.
To achieve these goals, the purification process of impurity in trimethyl orthoformate of the present invention, by the crude product trimethyl orthoformate pump delivery containing impurity, first after one-level paper element filtering device filters, enter from the bottom of resin mixed bed in resin mixed bed, impurity in crude product trimethyl orthoformate carries out exchange adsorption with resin in mixed bed, and the trimethyl orthoformate of removing impurity enters secondary paper element filtering device again from the upper end of resin mixed bed and filters; Its technology point is that crude product trimethyl orthoformate enters the flow control of resin mixed bed at 600-700L/h, and resin mixed bed temperature controls at 12 ~ 15 DEG C; Resin in described resin mixed bed adopts 330 weakly alkaline epoxy type anion exchange resins.
Another object of the present invention realizes like this, the specific equipment of impurity purifying in a kind of trimethyl orthoformate, it comprises resin mixed bed, the transfer lime that the upper end of resin mixed bed is provided with washings import and is connected with secondary paper element filtering device opening for feed, the transfer lime that the lower end of resin mixed bed is provided with washings outlet and is connected with one-level paper element filtering device discharge port, the opening for feed of described one-level paper element filtering device is connected with transferpump by pipeline; 330 weakly alkaline epoxy type anion exchange resins are filled in described resin mixed bed.
The specification of described resin mixed bed is Φ 400 × 3000.
Trimethyl orthoformate purification technique of the present invention, adopts mixed-bed resin to process, its foreign matter content can be dropped to less than 0.001%, even can't detect impurity by chromatogram.The invention solves prior art and there is the technical problem that dust removal rate is low, loss is many, cost is high.
accompanying drawing explanationaccompanying drawing is specific equipment structural representation of the present invention.
In figure 1, resin mixed bed 2, secondary paper element filtering device 3, one-level paper element filtering device 4, transferpump
embodimentthe purification process of impurity in trimethyl orthoformate of the present invention, by the crude product trimethyl orthoformate pump delivery containing impurity, first after one-level paper element filtering device filters, enter from the bottom of resin mixed bed in resin mixed bed, impurity in crude product trimethyl orthoformate carries out exchange adsorption with resin in mixed bed, and the trimethyl orthoformate of removing impurity enters secondary paper element filtering device again from the upper end of resin mixed bed and filters; Its key points for operation are that crude product trimethyl orthoformate enters the flow control of resin mixed bed at 650L/h, and resin mixed bed temperature controls at 13 DEG C; Resin in described resin mixed bed adopts 330 weakly alkaline epoxy type anion exchange resins.
With reference to accompanying drawing, the specific equipment of impurity purifying in trimethyl orthoformate of the present invention, it comprises resin mixed bed 1, the transfer lime that the upper end of resin mixed bed 1 is provided with washings import and is connected with secondary paper element filtering device 2 opening for feed, the transfer lime that the lower end of resin mixed bed 1 is provided with washings outlet and is connected with one-level paper element filtering device 3 discharge port, the opening for feed of described one-level paper element filtering device 3 is connected with transferpump 4 by pipeline; 330 weakly alkaline epoxy type anion exchange resins are filled in described resin mixed bed 1; The specification of described resin mixed bed 1 is Φ 400 × 3000.
The 330 weakly alkaline epoxy type anion exchange resins filled in processing requirement of the present invention and specification of equipment and resin mixed bed, be through that repeatedly orthogonal test proves repeatedly, selected device was through production practice in 2 years, after trimethyl orthoformate purifying, its foreign matter content drops to less than 0.001%, is " 0 " impurity N time with chromatogram detection.
Claims (1)
1. the purification process of impurity in a trimethyl orthoformate, it is characterized in that the crude product trimethyl orthoformate pump delivery containing impurity, first after one-level paper element filtering device filters, enter from the bottom of resin mixed bed in resin mixed bed, impurity in crude product trimethyl orthoformate carries out exchange adsorption with resin in mixed bed, and the trimethyl orthoformate of removing impurity enters secondary paper element filtering device again from the upper end of resin mixed bed and filters; Its technology point is that crude product trimethyl orthoformate enters the flow control of resin mixed bed at 600-700L/h, and resin mixed bed temperature controls at 12 ~ 15 DEG C; Resin in described resin mixed bed adopts 330 weakly alkaline epoxy type anion exchange resins.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210556889.2A CN103880616B (en) | 2012-12-19 | 2012-12-19 | The purification process of impurity and specific equipment thereof in trimethyl orthoformate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210556889.2A CN103880616B (en) | 2012-12-19 | 2012-12-19 | The purification process of impurity and specific equipment thereof in trimethyl orthoformate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103880616A CN103880616A (en) | 2014-06-25 |
| CN103880616B true CN103880616B (en) | 2016-01-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210556889.2A Active CN103880616B (en) | 2012-12-19 | 2012-12-19 | The purification process of impurity and specific equipment thereof in trimethyl orthoformate |
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| Country | Link |
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| CN (1) | CN103880616B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5922171A (en) * | 1997-01-24 | 1999-07-13 | Eco-Tec Limited | Method and apparatus for removing sodium chloride from pulping chemicals using an amphoteric ion-exchange resin |
| CN1431984A (en) * | 2000-06-02 | 2003-07-23 | 埃克森美孚化学专利公司 | Process for producing ultra-high purity isopropanol |
| CN101721885A (en) * | 2009-12-10 | 2010-06-09 | 攀枝花新钢钒股份有限公司 | Method for regenerating desulfurizer |
| CN201842708U (en) * | 2010-09-30 | 2011-05-25 | 杭州金枫叶科技有限公司 | Purifying device for online separation of metal salt and free acid in pickling solution |
| CN102701925A (en) * | 2012-06-26 | 2012-10-03 | 重庆紫光化工股份有限公司 | Method for purifying ortho-formate |
-
2012
- 2012-12-19 CN CN201210556889.2A patent/CN103880616B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5922171A (en) * | 1997-01-24 | 1999-07-13 | Eco-Tec Limited | Method and apparatus for removing sodium chloride from pulping chemicals using an amphoteric ion-exchange resin |
| CN1431984A (en) * | 2000-06-02 | 2003-07-23 | 埃克森美孚化学专利公司 | Process for producing ultra-high purity isopropanol |
| CN101721885A (en) * | 2009-12-10 | 2010-06-09 | 攀枝花新钢钒股份有限公司 | Method for regenerating desulfurizer |
| CN201842708U (en) * | 2010-09-30 | 2011-05-25 | 杭州金枫叶科技有限公司 | Purifying device for online separation of metal salt and free acid in pickling solution |
| CN102701925A (en) * | 2012-06-26 | 2012-10-03 | 重庆紫光化工股份有限公司 | Method for purifying ortho-formate |
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| Publication number | Publication date |
|---|---|
| CN103880616A (en) | 2014-06-25 |
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