CN1082510C - Process for synthesizing isomerol (isoether) phosphate - Google Patents
Process for synthesizing isomerol (isoether) phosphate Download PDFInfo
- Publication number
- CN1082510C CN1082510C CN99111755A CN99111755A CN1082510C CN 1082510 C CN1082510 C CN 1082510C CN 99111755 A CN99111755 A CN 99111755A CN 99111755 A CN99111755 A CN 99111755A CN 1082510 C CN1082510 C CN 1082510C
- Authority
- CN
- China
- Prior art keywords
- isomery alcohol
- phosphate ester
- ester salt
- ether
- phosphate
- 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.)
- Expired - Fee Related
Links
Abstract
The present invention relates to a method for synthesizing isomeric alcohol (ether) phosphate, which belongs to the technical field of organic compounds. Isomeric alcohol (ether) is used as a raw material, the phosphorylating synthesis reaction is carried out under the action of a phosphorylating reagent, and isomeric alcohol (ether) phosphate is prepared through hydrolysis and neutralization. The number of carbon atoms in the isomeric alcohol (ether) can be from 13 to 30. The phosphorylation reagent can be phosphorus pentoxide, pyrophosphoric acid, etc., and the molar ratio of the phosphorylation reagent to the isomeric alcohol (ether) is from 1: 2.1 to 3.5. The present invention has the characteristics of simple technology, mild reaction condition, favorable product color, favorable antistatic performance, favorable permeability, etc.
Description
The present invention relates to a kind of isomery alcohol phosphate ester salt synthetic method, belong to the preparing technical field of phosphate ester salt in the organic compound.
Phosphate ester salt is the important tensio-active agent of a class, with its excellent antistatic, emulsifying dispersivity, lubricated, washing and characteristic such as acidproof, alkaline-resisting, industrial circles such as textile of chemical fibre, leather plastics, papermaking, makeup have been widely used in, existing preparation to phosphate ester salt is a raw material with the alcohol of straight chained alkyl generally, under the phosphorylation agent effect, in phosphorylation reaction and hydrolysis,,, influenced the use properties and the quality product of phosphate ester salt owing to the difference on the molecular structure with synthetic.
The purpose of this invention is to provide a kind of is raw material with isomery alcohol, can effectively improve the synthetic method of the isomery alcohol phosphate ester salt of yield and product performance.
The present invention is an isomery alcohol phosphate ester salt synthetic method, is raw material with isomery alcohol, under the phosphorylation agent effect, isomery alcohol is carried out the phosphorylation building-up reactions, makes isomery alcohol phosphate ester salt through the hydrolysis neutralization again.
The fusing point and the viscosity of isomery alcohol are lower, and oxidative stability is good, have satisfactory stability and easy volatile, and the carbonatoms in the isomery alcohol of the present invention can be 13～30; Described phosphorylation agent can be Vanadium Pentoxide in FLAKES or tetra-sodium, phosphorus oxychloride, polyphosphoric acid etc.; The mol ratio of described phosphorylation agent and isomery alcohol can be 1: 2.1～and 3.5; Temperature of reaction in the described building-up reactions can be 45～85 ℃; Reaction times in the described building-up reactions can be 2～6 hours.
The present invention compared with prior art has the following advantages and positively effect:
1. the present invention makes the phosphorylation synthesis process simple because to adopt isomery alcohol be raw material, the yield height, and the reaction conditions gentleness, product color is good, and stable performance can effectively improve the collateralization degree of molecular structure, and facility investment and energy consumption are more saved.
2. by synthetic good product mobility of the present invention, viscosity is low, the raw material zero pour is low, compare with straight chained alkyl phosphate ester salt of the prior art, can significantly improve its static resistance, perviousness and wetting power, can be used as textile finish oil, synthon static inhibitor, softening agent, concrete high efficiency water reducing agent and farm chemical emulgent, be widely used.
Below in conjunction with embodiment the present invention is further described.
The embodiment of the invention is a raw material with isomery alcohol, and Vanadium Pentoxide in FLAKES (P is selected in phosphorylation trial-production for use
2O
5), the general molecular formula of described isomery alcohol is:
R is the straight chained alkyl of 8-20 carbon atom in the above-mentioned molecular formula
R ' is the straight chained alkyl of 1-10 carbon atom
Utilize the hydroxyl of isomery alcohol, can as the formula (1) esterification mainly take place with the phosphorylation agent Vanadium Pentoxide in FLAKES:
This esterification reaction product complexity the single, double ester in main production (1), also has a spot of three esters, poly phosphate and a part of inorganic phosphate by product to generate:
(three esters)
(poly phosphate)
H
3PO
4(inorganic phosphate) under less water and certain condition effect, poly phosphate can transform monoesters as the formula (2):
Under the effect of caustic alkali, monoesters in above-mentioned formula (1) and the formula (2) and dibasic acid esters carry out respectively obtaining isomery alcohol phosphate ester salt the finished product suc as formula the neutralization reaction of (3) and formula (4):
In formula (3) and (4), M is K, N
aIn basic metal.
Embodiment 1: in reactor, drops into 300 parts of (unit mole) isomery stearyl alcohol, under 70 ℃ temperature, slowly drops into 100 parts of Vanadium Pentoxide in FLAKESs (unit mole), reacted 4 hours, and under 70～80 ℃ temperature, the N with 30%
aThe neutralization of OH solution obtains isomery alcohol phosphoric acid ester sodium, is white thickness body.
Embodiment 2: drop into 250 parts of (unit mole) isomerous tridecanols in reactor, under 50 ℃ temperature, slowly drop into 100 parts of Vanadium Pentoxide in FLAKESs (unit mole), reacted 4 hours down at 55 ℃ then, under 50～70 ℃ temperature, KOH solution neutralization with 30% obtains isomery alcohol phosphate kalium salt, is little yellow thickness body.Isomery alcohol phosphate ester salt product of the present invention, its key technical indexes is: monoesters 50～60%; Dibasic acid esters: 40～50%; Total phosphorus: 4.4%, acid number 5～12mgkoh/g; 1% emulsion 24 hours is not stratified.
Claims (7)
1. an isomery alcohol phosphate ester salt synthetic method is characterized in that with isomery alcohol be raw material, under the phosphorylation agent effect, isomery alcohol is carried out the phosphorylation building-up reactions, makes isomery alcohol phosphate ester salt through the hydrolysis neutralization again.
2. by the described isomery alcohol of claim 1 phosphate ester salt synthetic method, it is characterized in that the carbonatoms in the described isomery alcohol can be 13～30.
3. by the described isomery alcohol of claim 1 phosphate ester salt synthetic method, it is characterized in that described phosphorylation agent can be Vanadium Pentoxide in FLAKES or tetra-sodium, phosphorus oxychloride, polyphosphoric acid.
4. by claim 1 or 2,3 described isomery alcohol phosphate ester salt synthetic methods, the mol ratio that it is characterized in that described phosphorylation agent and isomery alcohol is 1: 2.1～3.5.
5. by claim 1 or 2,3 described isomery alcohol phosphate ester salt synthetic methods, it is characterized in that the temperature of reaction in the described building-up reactions can be 45～85 ℃.
6. by claim 1 or 2,3 described isomery alcohol phosphate ester salt synthetic methods, it is characterized in that the reaction times in the described building-up reactions can be 2～6 hours.
7. by the described isomery alcohol of claim 4 phosphate ester salt synthetic method, it is characterized in that the temperature of reaction in the described building-up reactions can be 45～85 ℃, the reaction times can be 2～6 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99111755A CN1082510C (en) | 1999-08-08 | 1999-08-08 | Process for synthesizing isomerol (isoether) phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99111755A CN1082510C (en) | 1999-08-08 | 1999-08-08 | Process for synthesizing isomerol (isoether) phosphate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1247192A CN1247192A (en) | 2000-03-15 |
| CN1082510C true CN1082510C (en) | 2002-04-10 |
Family
ID=5275277
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99111755A Expired - Fee Related CN1082510C (en) | 1999-08-08 | 1999-08-08 | Process for synthesizing isomerol (isoether) phosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1082510C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831514A (en) * | 2010-05-15 | 2010-09-15 | 甘肃宏良皮业股份有限公司 | Method for preparing phosphate leather greasing agent |
| CN103374029A (en) * | 2013-06-04 | 2013-10-30 | 宁波市联凯化学有限公司 | Preparation method of fatty alcohol polyoxyethylene phosphate ester potassium salt |
| CN107827759B (en) * | 2016-06-29 | 2020-07-31 | 山东转化科技有限公司 | Alkylamine ether derived surfactant and preparation method thereof |
| CN114907902A (en) * | 2021-02-08 | 2022-08-16 | 联泓(江苏)新材料研究院有限公司 | Polyoxyethylene ether phosphate ester composition with high content of diester phosphate, and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1030245A (en) * | 1987-06-01 | 1989-01-11 | 阿姆奇姆产品公司 | Lubricated and the surface amendment of formed metal surfaces |
-
1999
- 1999-08-08 CN CN99111755A patent/CN1082510C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1030245A (en) * | 1987-06-01 | 1989-01-11 | 阿姆奇姆产品公司 | Lubricated and the surface amendment of formed metal surfaces |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1247192A (en) | 2000-03-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JPH0671546B2 (en) | Method for producing phosphate surfactant | |
| CN101456813A (en) | Method for synthesizing polyatomic alcohol fatty acid ester | |
| CN1082510C (en) | Process for synthesizing isomerol (isoether) phosphate | |
| US20020099234A1 (en) | Process for obtaining mixtures of phosphoric mono-and diesters | |
| CN103374029A (en) | Preparation method of fatty alcohol polyoxyethylene phosphate ester potassium salt | |
| EP0262227B1 (en) | Process for the preparation of myoinositol derivatives | |
| EP0613902A1 (en) | Process for the manufacture of poly(hydrocarbylene aryl phosphate)compositions | |
| CA1331627C (en) | Process for the continuous production of 2-phosphono-butane-1,2,4-tricarboxylic acid and alkali metal salts thereof | |
| CN101391956A (en) | Method for synthesizing methyl oleate and epoxy methyl oleate in ion liquid medium | |
| KR100252572B1 (en) | Process for the preparation of phosphoric monoester | |
| JPH07316170A (en) | Production of phosphoric monoester | |
| US4034023A (en) | Process for preparing mixed phosphate ester compositions | |
| CN112778124A (en) | Application of ionic liquid based on biimidazole in aspect of catalyzing biomass to prepare levulinic acid | |
| US4451410A (en) | Process for preparing condensed polyalkoxyphosphazene | |
| CN105713036A (en) | Preparation method of phosphomonoester | |
| US2693482A (en) | Preparation of alkene phosphonous acids | |
| EP0088359B1 (en) | Amidinophosphonic acids | |
| US4482506A (en) | Process for the manufacture of alkyl diaryl phosphate esters | |
| CA1155361A (en) | Process for preparing a pumpable surface-active product based on polyether acetic acid | |
| CN102807582A (en) | Preparation methods of organic phosphate ester and organic phosphate nucleating agent | |
| CA2066430C (en) | Process for the preparation of methylenebisphosphonic acids | |
| CN102875595A (en) | Preparation method of glyphosate | |
| CN109180725B (en) | Preparation method of alkynyl phosphate | |
| KR100281844B1 (en) | Method for producing bisstyryl fluorescent brightener | |
| CN1284512A (en) | Method of synthesizing atactic polyether fatty ester |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |