CN101665512A - Synthetic method of high-purity di-isooctyl acid phosphate - Google Patents
Synthetic method of high-purity di-isooctyl acid phosphate Download PDFInfo
- Publication number
- CN101665512A CN101665512A CN200910172333A CN200910172333A CN101665512A CN 101665512 A CN101665512 A CN 101665512A CN 200910172333 A CN200910172333 A CN 200910172333A CN 200910172333 A CN200910172333 A CN 200910172333A CN 101665512 A CN101665512 A CN 101665512A
- Authority
- CN
- China
- Prior art keywords
- warming
- incubated
- temperature
- hour
- esterification
- 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.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a synthetic method of high-purity di-isooctyl acid phosphate; phosphorus oxychloride is added in an esterification reaction kettle to carry out esterification reaction, and the whole esterification process is carried out in vacuum; esters are gradually added in the sodium hydroxide in an alkaline hydrolysis reaction kettle, and the mixture is still and layered; sodium hydroxide solution is added, the temperature is raised and the temperature is kept for half hour, and then still layering is carried out, alkaline cleaning is carried out for 2-3 times repeatedly; hydrochloric acid is added in an acidification reaction kettle, alkaline cleaning matters are gradually added and then the temperature is raised, and the temperature is kept for one hour and then still layering is carried out; and then the temperature of hydrochloric acid and water is raised, the temperature is raised, and then the temperature is kept for half hour, and still layering is carried out; byadopting the compound synthesized by the invention, under steam pressure, di-isooctyl acid phosphate with 95-97 percent of purity and isooctyl acid phosphate with 0.8-1.5 percent are respectively obtained after evaporation and condensation.
Description
Technical field
The present invention relates to a kind of synthetic method, especially a kind of synthetic method of high-purity di-isooctyl acid phosphate.
Background technology
At present, the synthetic many of domestic di (isooctyl) phosphate are main raw material with phosphorus oxychloride and isooctyl alcohol, realize through reactions such as esterification, alkaline hydrolysis, acidifyings, what the purifying of its last di (isooctyl) phosphate adopted is traditional underpressure distillation, material continuous high temperature in vacuum distillation process, long easily decomposition of time makes the purity of product low.
Summary of the invention
The present invention has proposed a kind of synthetic method of high-purity di-isooctyl acid phosphate for solving the low problem of product purity.
Technical scheme of the present invention: be through 1. esterification with di (isooctyl) phosphate; 2. alkaline hydrolysis; 3. acidifying; 4. isolation and purification four step process flow processs obtain the di (isooctyl) phosphate of purity at 95-97%, and the content of phosphoric acid one monooctyl ester is at 0.8-2.5%.
1. esterification: in reaction kettle of the esterification, add 450kg (about 2.85mol) phosphorus oxychloride, be cooled to below-5～20 ℃, drip 1000kg (about 7.60mol) isooctyl alcohol gradually, temperature of reaction is remained between 0～30 ℃, drip and finish insulation 1 hour, be warming up to 50-55 ℃, be incubated 2 hours, be warming up to 60-65 ℃ again, be incubated 4 hours, esterification finishes, the esterification whole process require vacuum tightness-0.080Mpa～-0.10Mpa between;
2. alkaline hydrolysis: add 42%～45% sodium hydroxide 1800kg (about 20.25mol) in the alkaline hydrolysis reactor, add carboxylate gradually, charge temperature is controlled at below 80 ℃, and reinforced end is warming up to 100-130 ℃, is incubated 2 hours, static layering; The sodium hydroxide solution 2000kg that adds 3-5% then is warming up to 90-95 ℃, is incubated half an hour, and static layering repeats alkali cleaning 2-3 time;
3. acidifying: in the acidification reaction still, add 20% hydrochloric acid 1000kg (about 5.48mol), be warming up to 60-65 ℃ after adding the alkali cleaning thing gradually, be incubated standing demix after 1 hour.Add entry 1500kg then, be warming up to 60-70 ℃, be incubated 0.5 hour, standing demix;
4. isolation and purification: after the acidifying, material charging under flow 300-600L/ hour speed, vapor pressure 0.2-0.5Mpa, vacuum tightness-0.096Mpa is above after evaporation, separation, condensation, obtain the di (isooctyl) phosphate of purity at 95-97%, the content of phosphoric acid one monooctyl ester is at 0.8-2.5%.
The invention has the beneficial effects as follows: adopt the present invention can obtain the di (isooctyl) phosphate of purity at 95-97%, the content of phosphoric acid one monooctyl ester is at 0.8-2.5%.
Embodiment
Following examples are used to illustrate the present invention, limit the scope of the invention but be not used in.
Embodiment 1:
1. esterification: in reaction kettle of the esterification, add the 450kg phosphorus oxychloride, be cooled to-5 ℃～below 20 ℃, drip the 1000kg isooctyl alcohol gradually, temperature of reaction is remained at below 0-30 ℃, drip and finish insulation 1 hour, be warming up to 50-55 ℃, be incubated 2 hours, be warming up to 60-65 ℃ again, be incubated 4 hours, esterification finishes, the esterification whole process require vacuum tightness-0.080Mpa～-0.10Mpa between;
2. alkaline hydrolysis: add 42～45% sodium hydroxide 1800kg in the alkaline hydrolysis reactor, add carboxylate gradually, temperature is controlled at below 80 ℃, and reinforced end is warming up to 100-130 ℃, is incubated 2 hours, static layering; The sodium hydroxide solution 2000kg that adds 3-5% then is warming up to 90-95 ℃, is incubated half an hour, and static layering repeats alkali cleaning 2-3 time;
3. acidifying: in the acidification reaction still, add 20% hydrochloric acid 1000kg, be warming up to 60-65 ℃ after adding the alkali cleaning thing gradually, be incubated standing demix after 1 hour.Add entry 1500kg then, be warming up to 60-70 ℃, be incubated 0.5 hour, standing demix;
4. isolation and purification: after the acidifying, material charging under flow 300-600L/ hour speed, vapor pressure 0.2-0.5Mpa, vacuum tightness-0.096Mpa～-0.10Mpa between after evaporation, separation, condensation, obtain the di (isooctyl) phosphate of purity at 95-97%, the content of phosphoric acid one monooctyl ester is at 0.8-2.5%.
Claims (1)
1, a kind of synthetic method of high-purity di-isooctyl acid phosphate is characterized in that:
1. esterification: in reaction kettle of the esterification, add 450kg (about 2.85mol) phosphorus oxychloride, be cooled to below-5～20 ℃, drip 1000kg (about 7.60mol) isooctyl alcohol gradually, temperature of reaction is remained between 0～30 ℃, drip and finish insulation 1 hour, be warming up to 50-55 ℃, be incubated 2 hours, be warming up to 60-65 ℃ again, be incubated 4 hours, esterification finishes, the esterification whole process require vacuum tightness-0.080Mpa～-0.10Mpa between;
2. alkaline hydrolysis: add 42%～45% sodium hydroxide 1800kg (about 20.25mol) in the alkaline hydrolysis reactor, add carboxylate gradually, charge temperature is controlled at below 80 ℃, and reinforced end is warming up to 100-130 ℃, is incubated 2 hours, static layering; The sodium hydroxide solution 2000kg that adds 3-5% then is warming up to 90-95 ℃, is incubated half an hour, and static layering repeats alkali cleaning 2-3 time;
3. acidifying: in the acidification reaction still, add 20% hydrochloric acid 1000kg (about 5.48mol), be warming up to 60-65 ℃ after adding the alkali cleaning thing gradually, be incubated standing demix after 1 hour.Add entry 1500kg then, be warming up to 60-70 ℃, be incubated 0.5 hour, standing demix;
4. isolation and purification: after the acidifying, material charging under flow 300-600L/ hour speed, vapor pressure 0.2-0.5Mpa, vacuum tightness-0.096Mpa is above after evaporation, separation, condensation, obtain the di (isooctyl) phosphate of purity at 95%-97%, the content of phosphoric acid one monooctyl ester is at 0.8-2.5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910172333A CN101665512A (en) | 2009-09-30 | 2009-09-30 | Synthetic method of high-purity di-isooctyl acid phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910172333A CN101665512A (en) | 2009-09-30 | 2009-09-30 | Synthetic method of high-purity di-isooctyl acid phosphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101665512A true CN101665512A (en) | 2010-03-10 |
Family
ID=41802314
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910172333A Pending CN101665512A (en) | 2009-09-30 | 2009-09-30 | Synthetic method of high-purity di-isooctyl acid phosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101665512A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104926863A (en) * | 2015-05-18 | 2015-09-23 | 河北科技大学 | Dibenzyl phosphate recovery method |
| CN105884821A (en) * | 2016-04-29 | 2016-08-24 | 三门峡中达化工有限公司 | Process for preparing bis phosphate from tri-iso-octyl phosphate by means of phosphonium salt phase-transfer catalytic hydrolysis |
| CN108997120A (en) * | 2018-07-04 | 2018-12-14 | 湖北犇星化工有限责任公司 | A kind of preparation method and its usage of isooctyl oleate |
| CN113717222A (en) * | 2021-08-30 | 2021-11-30 | 杭州潜阳科技股份有限公司 | Preparation method of high-purity dioctyl phosphate |
| CN113717222B (en) * | 2021-08-30 | 2024-06-04 | 杭州潜阳科技股份有限公司 | Preparation method of high-purity dioctyl phosphate |
-
2009
- 2009-09-30 CN CN200910172333A patent/CN101665512A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104926863A (en) * | 2015-05-18 | 2015-09-23 | 河北科技大学 | Dibenzyl phosphate recovery method |
| CN105884821A (en) * | 2016-04-29 | 2016-08-24 | 三门峡中达化工有限公司 | Process for preparing bis phosphate from tri-iso-octyl phosphate by means of phosphonium salt phase-transfer catalytic hydrolysis |
| CN108997120A (en) * | 2018-07-04 | 2018-12-14 | 湖北犇星化工有限责任公司 | A kind of preparation method and its usage of isooctyl oleate |
| CN113717222A (en) * | 2021-08-30 | 2021-11-30 | 杭州潜阳科技股份有限公司 | Preparation method of high-purity dioctyl phosphate |
| CN113717222B (en) * | 2021-08-30 | 2024-06-04 | 杭州潜阳科技股份有限公司 | Preparation method of high-purity dioctyl phosphate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102276464B (en) | Method for producing methyl acetoacetate | |
| CN102875594B (en) | Continuous synthesis technique of hydroxyethylidenediphosphonic acid | |
| CN101665512A (en) | Synthetic method of high-purity di-isooctyl acid phosphate | |
| WO2011040700A2 (en) | Method for producing alkyl lactate directly from ammonium lactate | |
| CN103467418A (en) | Method for preparing furan derivatives by catalytic conversion of fructose-based biomass | |
| CN105646580A (en) | Method for producing pentahydrate s-ornidazole disodium phosphate | |
| CN102911119A (en) | Preparation methods of 3,4-dimethyl pyrazole and 3,4-dimethyl pyrazole phosphate | |
| CN102276427B (en) | Method for preparing acetal from acrolein | |
| CN110862413A (en) | Glyphosate synthesis process and device | |
| CN102391113A (en) | Method for synthesizing trifluoropyruvate compound | |
| CN102229531B (en) | Preparation method of p-hydroxy benzal propane diacid derivative | |
| CN103044238B (en) | A kind of preparation method of racemic ketoprofen Isoleucine calcium | |
| CN107879987A (en) | A kind of preparation method of 2,3,5,6 Tetramethylpyrazine | |
| CN102391083A (en) | Method for synthesizing decyl acetal aldehyde | |
| CN101875673A (en) | Method for synthesizing glyphosate at low cost | |
| CN103204866A (en) | Production method of high purity triisopropyl borate | |
| CN101157608A (en) | Method for preparing 4-pentenoic acid | |
| CN102643177A (en) | Preparation method of aromatic hydrofluoroethers | |
| CN102442961A (en) | Production method of 1-methyl tetrazole | |
| CN101698632A (en) | High-purity 2-ethylene chlorohydrin production method | |
| CN103304411A (en) | Preparation method of malonic ester | |
| CN116655484B (en) | Preparation method of L-4-chloro-2-aminobutyric acid ester hydrochloride | |
| CN103804137A (en) | Method used for preparing higher alkanols via rice bran wax normal pressure reduction | |
| CN110862414B (en) | Process for catalytically synthesizing glyphosate | |
| CN101993454B (en) | Method for synthesizing tributyl phosphate by sodium formate acid-binding method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20100310 |