CN103724371A - Production method of high-content and low-trimethyl ester spermine - Google Patents
Production method of high-content and low-trimethyl ester spermine Download PDFInfo
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- CN103724371A CN103724371A CN201310697714.8A CN201310697714A CN103724371A CN 103724371 A CN103724371 A CN 103724371A CN 201310697714 A CN201310697714 A CN 201310697714A CN 103724371 A CN103724371 A CN 103724371A
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Abstract
The invention discloses a production method of high-content and low-trimethyl ester spermine, which comprises the following steps of: coarse amine water washing: washing a coarse amine compound with water in advance, and obtaining the coarse amine compound after water washing and lamination, and (2) high vacuum unit desolvation: conveying the coarse amine compound after the water washing and the lamination into a coarse amine compound head tank through a stock pump and then conveying the coarse amine compound into an evaporator for desolvation. According to the method, with the adoption of the coarse amine water washing, substance components in the coarse amine compound are simplified, the safety problem caused by pipeline blocking due to salt in a desolvation procedure is basically solved at the same time, the scaling probability due to concentration of ammonium chloride and ammonia scale in a vacuum pump in a desolvation process is greatly reduced, the product quality after desolvation can be ensured, furthermore, the production energy consumption is greatly reduced, and the maintenance expense is also greatly lowered.
Description
Technical field
The present invention relates to acephate technical field, the concrete production method that refers to the low trimethyl spermine of a kind of high-content.
Background technology
O, O-dimethyl thiophosphoryl amide (hereinafter to be referred as spermine) is the main intermediate of producing high-efficiency low-toxicity organophosphorus pesticide acephate.
Acephate belongs to a kind of water-soluble broad spectrum insecticide, miticide, has stomach toxicity, tags and systemic action, can be used for preventing and treating the various pests of the crops such as paddy rice, corn, cotton.Also can be used for vegetable crop, cotton, Caulis et Folium Brassicae capitatae and potato etc.Its insecticidal mechanism is the activity that suppresses Pseudocholinesterase in pest body.The history that has had decades in domestic product and application.So far, acephate remains the Pesticidal products of large-tonnage production and selling on world market, and annual turnover is more than 400,000,000 dollars.
Home products structure is comparatively single at present, for expanding market sale, enriches the structure (newly-increased 97% spermine specification) of product, and the production method of the low trimethyl spermine of research high-content is the demand in market.
Summary of the invention
The production method that the object of this invention is to provide the low trimethyl spermine of a kind of high-content, specifically refers to O, and O-dimethyl thiophosphoryl amide is produced the method containing low trimethyl spermine when precipitation, and the method technical process is simple, easy to operate, and production energy consumption is low.
For achieving the above object, the production method of the low trimethyl spermine of high-content provided by the invention, it comprises the steps:
(1) thick amine washing: in advance thick aminate is washed, the mode of thick amine washing is that thick aminate and water are fully dissolved and entered multi_layer extraction after water-and-oil separator after mixed by transfering material pump, obtains washing the thick aminate after layering; And the aminate dissolving in the rear waste water of thick amine washing is reclaimed in extraction;
(2) high vacuum unit precipitation: the thick aminate after washing layering is pumped to by getting the raw materials ready in thick aminate header tank, thicker aminate is delivered to precipitation in vaporizer; The thick aminate flow that adjusting enters vaporizer is 1300～1500L/h, the vacuum keep in vaporizer-more than 0.095Mpa, the liquid temperature of controlling material in vaporizer is 120～126 ℃, controlling temperature is 85～95 ℃.
As preferred version, in described step (1), by transfering material pump, being undertaken fully dissolving mixed thick aminate and discharge ratio is 1:2～3.
Further, the thick aminate flow that the middle adjusting of described step (2) enters vaporizer is 1400L/h, and the liquid temperature of controlling material in vaporizer is 124 ℃, and controlling temperature is 90 ℃.
For producing the spermine product of high-content, low trimethyl, must first to crude product aminate (being called for short thick amine), wash, remove most salt and inorganic ammonia wherein, simplify material component, be convenient to separation; Then under the condition of high vacuum, carry out precipitation, remove trimethyl and other impurity.Method of the present invention, the thick aminate that amination operation is produced is by after washing, remove most of salt (ammonium chloride) and inorganic ammonia wherein, then enter into the precipitation system of condition of high vacuum degree, remove moisture content, trimethyl and partial impurities, obtain the spermine product that main content is high, trimethyl is low.
The invention has the advantages that: the material component in thick aminate has not only been simplified in the thick amine washing of method of the present invention, fundamentally solved the safety problem that precipitation operation produces because of salt blocking pipe sometimes simultaneously, and significantly reduced desolvation process intermediate pump ammonium chloride and ammonia dirt and concentrated at fouling probability in vacuum pump, quality product after precipitation can be guaranteed, and also reduction greatly of production energy consumption, maintenance cost also declines to a great extent.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment mono-:
The production method of the low trimethyl spermine of high-content of the present invention, implementation step is as follows:
(1) thick amine washing: in advance thick aminate is washed, the mode of thick amine washing is, and by thick aminate and water, according to flow proportional, to be 1:2 fully dissolved and entered multi_layer extraction after water-and-oil separator after mixed by transfering material pump, obtains washing the thick aminate after layering; And the aminate dissolving in the rear waste water of thick amine washing is reclaimed in extraction.
(2) high vacuum unit precipitation: the thick aminate after washing layering is pumped to by getting the raw materials ready in thick aminate header tank, thicker aminate is delivered to precipitation in vaporizer; The thick aminate flow that adjusting enters vaporizer is 1300L/h, the vacuum keep in vaporizer-more than 0.095Mpa, the liquid temperature of controlling material in vaporizer is 120 ℃, controlling temperature is 85 ℃.
After precipitation, the indices of spermine is as follows: the main content > 97% of spermine, water content < 0.2%, trimethyl content < 2.4%, ammonium chloride content < 0.4%.
Embodiment bis-:
Procedure is with embodiment mono-, difference is: (1) thick amine washing: in advance thick aminate is washed, the mode of thick amine washing is, and by thick aminate and water, according to flow proportional, to be 1:2.5 fully dissolved and entered multi_layer extraction after water-and-oil separator after mixed by transfering material pump; (2) high vacuum unit precipitation: the thick aminate flow that adjusting enters vaporizer is 1400L/h, the liquid temperature of controlling material in vaporizer is 124 ℃, controlling temperature is 90 ℃.
After precipitation, the indices of spermine is as follows: the main content > 97.5% of spermine, water content < 0.2%, trimethyl content < 2.2%, ammonium chloride content < 0.1%.
Embodiment tri-:
Procedure is with embodiment mono-, and difference is:
(1) thick amine washing: in advance thick aminate is washed, the mode of thick amine washing is, and to be 1:3 by thick aminate and water according to flow proportional fully dissolved and entered multi_layer extraction after water-and-oil separator after mixed by transfering material pump; (2) high vacuum unit precipitation: the thick aminate flow that adjusting enters vaporizer is 1500L/h, the liquid temperature of controlling material in vaporizer is 126 ℃, controlling temperature is 95 ℃.
After precipitation, the indices of spermine is as follows: the main content > 97.2% of spermine, water content < 0.3%, trimethyl content < 2.1%, ammonium chloride content < 0.4%.
Principle of work of the present invention is as follows:
(1) thick amine washing: owing to can following the generation of a large amount of inorganic salt and the appearance of other organic by-products in the process producing thick aminate, the component relative complex in therefore thick aminate.Excessive inorganic ammonia when removing a large amount of inorganic salt (ammonium chloride) wherein and reaction, must wash thick aminate in advance, and during for precipitation, being convenient to separation provides prerequisite.For reducing the loss in thick amine water washing process, workshop increases an extraction tower newly simultaneously.The use of extraction tower is mainly the aminate dissolving in the rear waste water of thick amine washing in order to reclaim.The mode of thick amine washing be by thick aminate and water according to a certain percentage (flow) by transfering material pump, fully dissolve and enter the object that multi_layer extraction after water-and-oil separator reaches washing after mixed.The material component in thick aminate has not only been simplified in thick amine washing, has fundamentally solved the safety problem that precipitation operation produces because of salt blocking pipe sometimes simultaneously.
(2) high vacuum unit precipitation: in the thick amine after washing, the content of ammonium chloride declines to a great extent, this type of incondensable gas of inorganic ammonia reduces simultaneously, so just significantly reduce desolvation process intermediate pump ammonium chloride and ammonia dirt and concentrated at fouling probability in vacuum pump, Roots-back and forth high-vacuum pump unit can move under operating mode preferably, just can guarantee to realize low trimethyl spermine and produce.My subsidiary factory utilizes a Roots-reciprocal high-vacuum pump unit (JZJW300-22) to carry out production run at first set precipitation device, and the cycle of operation has reached four months at present, and unit operation in order.Not only the quality product after precipitation can be guaranteed, and can reach customer requirement completely, and production energy consumption is than also greatly reducing in the past, and maintenance cost also declines to a great extent.This way is worth further in precipitation system, promoting.
After crude product aminate (dimethyl thiophosphoryl amide) is washed, through thin-film evaporator, under the condition of high vacuum, produce the spermine product of content high (being greater than 97%), trimethyl low (being less than 2.4%).
Claims (3)
1. a production method for the low trimethyl spermine of high-content, it comprises the steps:
(1) thick amine washing: in advance thick aminate is washed, the mode of thick amine washing is that thick aminate and water are fully dissolved and entered multi_layer extraction after water-and-oil separator after mixed by transfering material pump, obtains washing the thick aminate after layering; And the aminate dissolving in the rear waste water of thick amine washing is reclaimed in extraction;
(2) high vacuum unit precipitation: the thick aminate after washing layering is pumped to by getting the raw materials ready in thick aminate header tank, thicker aminate is delivered to precipitation in vaporizer; The thick aminate flow that adjusting enters vaporizer is 1300～1500L/h, the vacuum keep in vaporizer-more than 0.095Mpa, the liquid temperature of controlling material in vaporizer is 120～126 ℃, controlling temperature is 85～95 ℃.
2. the production method of the low trimethyl spermine of high-content according to claim 1, is characterized in that: in described step (1), by transfering material pump, being undertaken fully dissolving mixed thick aminate and discharge ratio is 1:2～3.
3. the production method of the low trimethyl spermine of high-content according to claim 1 and 2, it is characterized in that: the thick aminate flow that the middle adjusting of described step (2) enters vaporizer is 1400L/h, the liquid temperature of controlling material in vaporizer is 124 ℃, and controlling temperature is 90 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310697714.8A CN103724371A (en) | 2013-12-18 | 2013-12-18 | Production method of high-content and low-trimethyl ester spermine |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310697714.8A CN103724371A (en) | 2013-12-18 | 2013-12-18 | Production method of high-content and low-trimethyl ester spermine |
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| CN103724371A true CN103724371A (en) | 2014-04-16 |
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| CN201310697714.8A Pending CN103724371A (en) | 2013-12-18 | 2013-12-18 | Production method of high-content and low-trimethyl ester spermine |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112552337A (en) * | 2020-12-10 | 2021-03-26 | 安道麦股份有限公司 | Production method of high-purity spermine and coproduction of high-purity trimethyl thiophosphate byproduct |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486731A (en) * | 2008-12-12 | 2009-07-22 | 荆州市沙市东方有机化工研究所 | Production method of O, O-dimethyl thiophosphoryl chloride |
| CN102060871A (en) * | 2010-12-13 | 2011-05-18 | 浙江嘉化集团股份有限公司 | Method for separating and purifying by-product trimethyl thiophosphate |
-
2013
- 2013-12-18 CN CN201310697714.8A patent/CN103724371A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486731A (en) * | 2008-12-12 | 2009-07-22 | 荆州市沙市东方有机化工研究所 | Production method of O, O-dimethyl thiophosphoryl chloride |
| CN102060871A (en) * | 2010-12-13 | 2011-05-18 | 浙江嘉化集团股份有限公司 | Method for separating and purifying by-product trimethyl thiophosphate |
Non-Patent Citations (2)
| Title |
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| 余金林: "生产高纯度精胺的方法研究", 《PESTICIDES》 * |
| 艾秋红等: "O,O-二甲基硫代磷酰氯氨解过程废物最小化", 《化工进展》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112552337A (en) * | 2020-12-10 | 2021-03-26 | 安道麦股份有限公司 | Production method of high-purity spermine and coproduction of high-purity trimethyl thiophosphate byproduct |
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