CN210252272U - Production device of phosphonic acid tris (1, 3-dichloropropyl) ester - Google Patents
Production device of phosphonic acid tris (1, 3-dichloropropyl) ester Download PDFInfo
- Publication number
- CN210252272U CN210252272U CN201920948105.8U CN201920948105U CN210252272U CN 210252272 U CN210252272 U CN 210252272U CN 201920948105 U CN201920948105 U CN 201920948105U CN 210252272 U CN210252272 U CN 210252272U
- Authority
- CN
- China
- Prior art keywords
- reaction tower
- dichloropropyl
- reaction
- towers
- stage
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Abstract
The utility model discloses a production device of phosphonic acid tris (1, 3-dichloropropyl) ester. The utility model discloses a: the device comprises two dropwise adding tanks filled with raw materials, three reaction towers and a material collecting kettle, wherein the three reaction towers are connected in sequence, the bottom parts of the dropwise adding tanks A and B are respectively connected with a feed inlet of a first-stage reaction tower, the discharge outlets of the previous reaction tower are connected with a feed inlet of the next reaction tower, and pipelines connected in series with the three reaction towers are all connected in series with a control valve and a material transferring pump; the bottom discharge ports of the dripping tank A and the dripping tank B are connected with the feed inlet of the first-stage reaction tower through pipelines, and control valves and mass flowmeters are connected on the pipelines in series; the discharge hole of the third-stage reaction tower is connected with the feed inlet at the top of the material collection kettle through a pipeline b, and the fillers in the three reaction towers are solid catalysts.
Description
Technical Field
The utility model relates to a fine chemical equipment field for synthesizing phosphonic acid tris (1, 3-dichloro-2-propyl) ester by using phosphorus oxychloride and dichloropropanol as raw materials and solid super acid as a catalyst.
Background
The phosphonic acid tri (1, 3-dichloro-2-propyl) ester is an additive type general chlorine-containing phosphorus-containing flame retardant, has flame retardant, plasticizing, damp-proof, static interference, tensile resistance and compression resistance, and halogen atoms generated by decomposition at high temperature have the function of trapping active free radicals in combustion so as to enable high-activity hydroxyl or hydrogen atoms to generate water or hydrogen, thereby interrupting chain oxidation reaction. Therefore, tris (1, 3-dichloro-2-propyl) phosphonate is widely used as a good flame retardant and flame retardant plasticizer for unsaturated polyesters, rigid and flexible polyurethane foams, epoxy resins, phenolic resins, flexible polyvinyl chloride, and the like.
Disclosure of Invention
In order to provide a phosphonic acid tris (1, 3-dichloro-2-propyl) ester production device which has simple equipment structure, is easy to operate, can effectively improve the equipment utilization rate and the reaction efficiency, realizes the continuous production of phosphonic acid tris (1, 3-dichloro-2-propyl) ester, and is safe and energy-saving. The utility model adopts the technical scheme as follows:
an apparatus for producing tris (1, 3-dichloropropyl) phosphonate, comprising: the device comprises two dropwise adding tanks filled with raw materials, three reaction towers and a material collecting kettle, wherein the three reaction towers are connected in sequence, the bottom parts of the dropwise adding tanks A and B are respectively connected with a feed inlet of a first-stage reaction tower, the discharge outlets of the previous reaction tower are connected with a feed inlet of the next reaction tower, and pipelines connected in series with the three reaction towers are all connected in series with a control valve and a material transferring pump;
the bottom discharge ports of the dripping tank A and the dripping tank B are connected with the feed inlet of the first-stage reaction tower through pipelines, and control valves and mass flowmeters are connected on the pipelines in series; the discharge hole of the third-stage reaction tower is connected with the feed inlet at the top of the material collection kettle through a pipeline b, and the fillers in the three reaction towers are solid catalysts.
According to the production device of the phosphonic acid tris (1, 3-dichloropropyl) ester, the discharge ports at the top of each stage of reaction tower are connected with a gas absorption device through a pipeline a.
According to the production device of the phosphonic acid tris (1, 3-dichloropropyl) ester, a discharge hole of the third-stage reaction tower is connected with a feed hole of the third-stage reaction tower through a pipeline c, and a control valve and a material transfer pump are connected in series on the pipeline c.
According to the production device of the phosphonic acid tris (1, 3-dichloropropyl) ester, the three reaction towers which are sequentially connected are all made of stainless steel.
According to the production device of the phosphonic acid tris (1, 3-dichloropropyl) ester, the fillers in the three reaction towers are all strong-acid cationic resin catalysts which are soaked and activated by 1, 3-dichloropropanol.
According to the production device of the phosphonic acid tris (1, 3-dichloropropyl) ester, the two dripping tanks and the material collecting kettle are made of one of ceramic, stainless steel or ceramic-lined polytetrafluoroethylene.
The utility model discloses technical scheme has following characteristics:
the device adopts the solid catalyst required by the reaction as the basic filler of the reaction tower, has simple equipment structure, is easy to operate, effectively improves the equipment utilization rate and the reaction efficiency, is easy to realize the continuous production of the phosphonic acid tris (1, 3-dichloro-2-propyl) ester, and is safe and energy-saving.
The device mainly comprises a raw material dripping tank, 1-3 stages of catalytic reaction towers and a material collecting kettle, wherein each stage of reaction tower is connected end to end, and a control valve and a material transferring pump are connected in series on connected pipelines. The novel device has simple structure and easy operation, can effectively improve the utilization rate and the reaction efficiency of equipment, and realizes the continuous production, safety and energy conservation of the tris (1, 3-dichloro-2-propyl) phosphonate.
Drawings
FIG. 1 is a schematic diagram of the production line of tris (1, 3-dichloropropyl) phosphonate.
In the drawings: 1. a first-stage reaction tower; 2. a secondary reaction tower; 3. a third-stage reaction tower; 4. a dropping tank A; 5. a dropping tank B; 6. a mixing pump; 7. a material collection kettle; 101. a feed inlet of the first-stage reaction tower; 102. a discharge hole of the first-stage reaction tower; 103. packing in the reaction tower; 104. a discharge hole at the top of the first-stage reaction tower; 201. a feed inlet of the secondary reaction tower; 202. a discharge hole at the top of the secondary reaction tower; 203. a discharge hole of the secondary reaction tower; 301. a feed inlet of the third-stage reaction tower; 302. a discharge hole at the top of the third-stage reaction tower; 303. a discharge hole of the third-stage reaction tower; 701. a top feed port; 702. a bottom discharge hole.
Detailed Description
The present invention will be further explained with reference to fig. 1.
The utility model relates to a production device of phosphonic acid tris (1, 3-dichloro-2-propyl) ester, include: three reaction towers, two dropwise add jars that are equipped with the raw materials, material collection cauldron 7 that connect gradually, three reaction tower all are provided with reaction tower feed inlet, reaction tower top discharge gate at the top, are provided with the reaction tower discharge gate in the bottom.
The discharge ports at the bottoms of the dripping tank A and the dripping tank B are respectively connected with the feed inlet 101 of the first-stage reaction tower through pipelines. The three reaction towers are connected in sequence, the bottom discharge hole of the previous reaction tower is connected with the reaction tower feed inlet of the next reaction tower, and the three reaction tower series pipelines are all connected in series with a control valve and a material transfer pump. The discharge gate and the one-level reaction tower feed inlet 101 of dropwise add jar A and dropwise add jar B bottom are all established through the pipeline and are connected, all establish ties on the branch pipeline of dropwise add jar bottom and have control valve, mass flow meter, install compounding pump 6 on the pipeline that one-level reaction tower feed inlet 101 is connected.
The discharge ports at the tops of the three reaction towers are all connected with a gas absorption device through a pipeline a to discharge hydrogen chloride byproducts; the bottom discharge ports 303 of the three reaction towers are connected with the top feed port 701 of the material collection kettle through a pipeline b, and the pipeline b is provided with a control valve and a material transfer pump. The discharge port 303 of the third-stage reaction tower is connected with the feed port 301 of the third-stage reaction tower through the pipeline c, and when the reaction conversion rate is low, the material discharged from the discharge port 303 of the third-stage reaction tower can be returned to the third-stage reaction tower through the feed port 301 of the third-stage reaction tower through the pipeline c to continue the esterification reaction. The pipeline c is connected in series with a valve and a material transferring pump.
The first to third reaction towers are made of stainless steel. The packing in the first to third stages of reaction towers is a solid catalyst required by the reaction. The material of the raw material dripping tank A, the material dripping tank B and the material collecting kettle 7 can be one of ceramic, stainless steel or ceramic-lined polytetrafluoroethylene material.
The utility model discloses a working process:
respectively pumping the metered material phosphorus oxychloride and 1, 3-dichloropropanol into a ceramic material dropwise adding tank A and a ceramic material dropwise adding tank B which are 1000m in specification, continuously pumping into a first-stage reaction tower through a feed inlet of the first-stage reaction tower at a constant speed by a mixing pump 6 according to a set flow rate, then entering a second-stage reaction tower through a discharge outlet 102 of the first-stage reaction tower, and then entering a feed inlet at the top of the third-stage reaction tower through a discharge outlet 203 of the second-stage reaction tower to enter a third-stage reaction tower. The reaction mixture is monitored by gas phase central control, and when the esterification conversion rate is less than 95%, the material discharged from the discharge hole 303 of the third-stage reaction tower returns to the third-stage reaction tower through the feed hole 301 of the third-stage reaction tower through the pipeline c to continue the esterification reaction.
The content of the phosphonic acid tris (1, 3-dichloro-2-propyl) ester in the esterification product is monitored by a gas chromatograph under the detection condition of the gas chromatograph, namely the temperature of a gasification chamber is 240 ℃, and N is2The total purging flow is 23.0mL/min, the gas flow in the chromatographic column is 3.0mL/min, the chromatographic column is a capillary column with the column length of 30m, the temperature of a hydrogen flame detector is 280 ℃, and the esterification conversion rate of the reaction materials is calculated according to the content of the tris (1, 3-dichloro-2-propyl) phosphonate, wherein the specific esterification conversion rate calculation method comprises the following steps:
wherein: m is1-total mass of reaction mixture, kg;
c- - -gas chromatography content,%, of the product in the reaction mixture;
m1-the feed of phosphorus trichloride before the reaction, kg;
153.5- -phosphorus oxychloride molar mass, g/mol;
431- - -tris (1, 3-dichloro-2-propyl) phosphonate in molar mass, g/mol.
When the esterification conversion rate of the reaction mixture is more than 95% by gas phase central control monitoring, the material from the discharge port 303 of the third-stage reaction tower enters a material collecting kettle through a pipeline b through a top feed port 701, and is subjected to alkali washing, water washing and distillation treatment to obtain a qualified product, namely tris (1, 3-dichloro-2-propyl) phosphonate, and then the qualified product is pumped into a finished product tank through a bottom discharge port 702. Wherein, the packing 103 in the stainless steel reaction tower from one to three stages is a strong acid cation resin catalyst which is soaked and activated by 1, 3-dichloropropanol. Hydrogen chloride gas generated by the reaction of each reaction tower respectively enters the negative pressure tail gas absorption device through a discharge hole at the top of the first-stage reaction tower, a discharge hole at the top of the second-stage reaction tower and a discharge hole at the top of the third-stage reaction tower through a pipeline a for treatment. Wherein the control ranges of the temperature in the first-stage reaction tower to the third-stage reaction tower are respectively 115-118 ℃, 126-130 ℃ and 135-138 ℃.
The above-mentioned embodiments are only described for the preferred embodiments of the present invention, and are not intended to limit the concept and scope of the present invention, and the ordinary engineers in this field should fall into the scope of the present invention for various modifications and improvements of the technical solution of the present invention without departing from the design concept of the present invention.
Claims (6)
1. A production device of phosphonic acid tris (1, 3-dichloropropyl) ester is characterized in that:
the method comprises the following steps: the device comprises two dropwise adding tanks filled with raw materials, three reaction towers and a material collecting kettle (7), wherein the three reaction towers are connected in sequence, the discharge ports at the bottoms of the dropwise adding tanks A and B are connected with the feed port (101) of the first-stage reaction tower, the discharge port of the previous reaction tower is connected with the feed port of the next reaction tower, and pipelines connected in series with the three reaction towers are all connected in series with a control valve and a material transferring pump;
the bottom discharge ports of the dripping tank A and the dripping tank B are connected with the feed port (101) of the first-stage reaction tower through pipelines, and control valves and mass flowmeters are connected on the pipelines in series; the discharge hole (303) of the three-stage reaction tower is connected with the top feed inlet (701) of the material collection kettle (7) through a pipeline b, and the fillers in the three reaction towers are solid catalysts.
2. The apparatus for producing tris (1, 3-dichloropropyl) phosphonate in accordance with claim 1, wherein: and the discharge ports at the top of each stage of reaction tower are connected with a gas absorption device through pipelines a.
3. The apparatus for producing tris (1, 3-dichloropropyl) phosphonate in accordance with claim 1, wherein: the discharge hole (303) of the third-stage reaction tower is also connected with the feed hole (301) of the third-stage reaction tower through a pipeline c, and a control valve and a material transferring pump are connected in series on the pipeline c.
4. The apparatus for producing tris (1, 3-dichloropropyl) phosphonate in accordance with claim 1, wherein: and the three reaction towers which are sequentially connected are all made of stainless steel.
5. The apparatus for producing tris (1, 3-dichloropropyl) phosphonate in accordance with claim 1, wherein: the fillers in the three reaction towers are all strong acid cation resin catalysts which are soaked and activated by 1, 3-dichloropropanol.
6. The apparatus for producing tris (1, 3-dichloropropyl) phosphonate in accordance with claim 1, wherein: the two dripping tanks and the material collecting kettle are made of one of ceramics, stainless steel or ceramic-lined polytetrafluoroethylene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920948105.8U CN210252272U (en) | 2019-06-24 | 2019-06-24 | Production device of phosphonic acid tris (1, 3-dichloropropyl) ester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920948105.8U CN210252272U (en) | 2019-06-24 | 2019-06-24 | Production device of phosphonic acid tris (1, 3-dichloropropyl) ester |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN210252272U true CN210252272U (en) | 2020-04-07 |
Family
ID=70044158
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201920948105.8U Active CN210252272U (en) | 2019-06-24 | 2019-06-24 | Production device of phosphonic acid tris (1, 3-dichloropropyl) ester |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN210252272U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110511239A (en) * | 2019-09-24 | 2019-11-29 | 山东泰和水处理科技股份有限公司 | A kind of production method of phosphonic acids three (bis- chloropropyl of 1,3-) ester |
-
2019
- 2019-06-24 CN CN201920948105.8U patent/CN210252272U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110511239A (en) * | 2019-09-24 | 2019-11-29 | 山东泰和水处理科技股份有限公司 | A kind of production method of phosphonic acids three (bis- chloropropyl of 1,3-) ester |
| WO2021057207A1 (en) * | 2019-09-24 | 2021-04-01 | 山东泰和水处理科技股份有限公司 | Method for producing tris(1,3-dichloropropyl)phosphate |
| CN110511239B (en) * | 2019-09-24 | 2021-12-31 | 山东泰和水处理科技股份有限公司 | Production method of tris (1, 3-dichloropropyl) phosphonate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103333047B (en) | Preparation method of dichloropropanol | |
| CN102898311A (en) | Method and equipment for continuously producing methyl nitrite | |
| CN210252272U (en) | Production device of phosphonic acid tris (1, 3-dichloropropyl) ester | |
| CN104370740B (en) | Compounding acetic isoborneol ester production method | |
| CN105348228B (en) | Method and device for industrially and continuously producing tetrahydrofurfuryl alcohol diethyl ether | |
| CN104209144B (en) | The preparation method of a kind of catalyst system and catalyzing and preparation method thereof and vinylacetylene | |
| CN102924271B (en) | Method for producing tert-butyl ester compound by performing esterification reaction, rectification and coupling to organic carboxylic acid and isobutene | |
| CN102464546B (en) | Double-tower depropanization process for reducing reboiler scaling | |
| CN105523982A (en) | Method for preparing tert-butyl hydroperoxide | |
| CN208182885U (en) | A kind of novel reaction equipment prepared to benzyl dichloride | |
| CN211111803U (en) | Dimethyl phosphite apparatus for producing | |
| CN101671224B (en) | Preparation method of high purity dicyclopentadiene | |
| CN204275801U (en) | Breather pipe bubble type acetylene gas purifier | |
| CN203728742U (en) | Equipment for preparing chloropivaloyl pentane | |
| WO2021057207A1 (en) | Method for producing tris(1,3-dichloropropyl)phosphate | |
| CN203440262U (en) | Device for producing trans-1, 2-dichloroethylene with acetylene by adopting catalytic chlorination method | |
| CN103819380A (en) | New method for producing p-menthane hydroperoxide with series connection of multiple bubbling-tower reactors | |
| CN211302119U (en) | Device for preparing polymer-grade isobutene by catalytic distillation method | |
| CN1793093A (en) | Process for preparing 1,1,2 trichloroethylane | |
| CN103936548B (en) | A kind of method of 1,2-ethylene dichloride chlorination production vinyl trichloride | |
| CN209368156U (en) | Mixed butyl alcohol adds the device of hydrogen in a kind of butyl octanol unit | |
| CN202185160U (en) | Methanol recovery and distillation kettle for preparation of calcium acetylacetonate | |
| CN202924736U (en) | Novel device for producing phosphorus oxychloride | |
| CN211302122U (en) | Ethylene by-product C9 raw materials processing system | |
| CN203768006U (en) | Energy-saving type circulating CO change device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: No.1, Shiliquan East Road, Shizhong District, Zaozhuang City, Shandong Province 277100 Patentee after: Shandong Taihe Technology Co.,Ltd. Address before: No.1, Shiliquan East Road, Shizhong District, Zaozhuang City, Shandong Province 277100 Patentee before: SHANDONG TAIHE WATER TREATMENT TECHNOLOGIES Co.,Ltd. |