CN106632739A - Phosphate emulsifier and preparation method thereof - Google Patents
Phosphate emulsifier and preparation method thereof Download PDFInfo
- Publication number
- CN106632739A CN106632739A CN201611133213.7A CN201611133213A CN106632739A CN 106632739 A CN106632739 A CN 106632739A CN 201611133213 A CN201611133213 A CN 201611133213A CN 106632739 A CN106632739 A CN 106632739A
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- CN
- China
- Prior art keywords
- parts
- phosphorus pentoxide
- polyethenoxy ether
- alcohol polyethenoxy
- class compound
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
Abstract
A phosphate emulsifier is composed of the following components in parts by weight: 85 to 95 parts of isomeric alcohol ethoxylate compounds, 0.1 to 0.5 part of hypophosphorous acid solution (50%), 5 to 15 parts of phosphorus pentoxide (P2O5), 0.1 to 0.5 part of hydrogen peroxide solution (35%), and 0.1 to 2 parts of deionized water. The isomeric alcohol ethoxylate compounds have a structural formula: R1O-(C2H4O)n-R2, R1 is a C10 or C13 isomeric alkyl, R2 is a hydrogen atom or an organic residue, and n represents the number of EO and is one of 2-3, 5-6, 8-10, 12, and 15. The raw material cost is low, thus the emulsifier is cheap and economic, the application range of the emulsifier is wide; moreover, the emulsifier does not contain any formaldehyde, and is safe and environment-friendly; the stability is good, the emulsifying effect is good, the particle size of emulsified substance becomes smaller, the particle size distribution is more even, the gel is less after emulsification, and the corrosion resistance, thermal stability, and optical stability of polymer film are all improved.
Description
Technical field
The present invention relates to a kind of phosphate emulsifying agent and preparation method thereof, belongs to emulsifying agent field.
Background technology
Emulsifying agent is can to improve the various surface tension constituted between phase in emulsion, is allowed to form uniform and stable dividing
Prose style free from parallelism system or the material of emulsion.Emulsifying agent is surface reactive material, has hydrophilic group and lipophilic group in molecule simultaneously, and it assembles
On oil/water interface, interfacial tension can be reduced and reduced to form energy required for emulsion, so as to improve the energy of emulsion
Amount.
Phosphate emulsifying agent can be used to extensively prepare as pure third, and the emulsion polymer such as second third and phenylpropyl alcohol is particularly a kind of
The preparation of ink pigments mill base pre-emulsion, these polymer can apply to emulsion paint, adhesive, coating for paper and textile industry
In, pre-emulsion can be used for the preparation of ink pigments mill base.Existing some emulsifier preparation method is more complicated, preparation cost
Height, and the emulsifying effectiveness of the emulsifying agent for obtaining is not ideal enough, stability is poor, and some are even also containing the materials such as formaldehyde, inadequate ring
Protect.So needing a kind of relatively cheap, good stability, the emulsifying agent of safety and environmental protection.
The content of the invention
To solve an existing difficult problem above, the invention discloses a kind of phosphate emulsifying agent and preparation method thereof.
A kind of phosphate emulsifying agent, is made up of the component of following mass fraction：Isomeric alcohol polyethenoxy ether class compound 85-
95 parts, 50% hypophosphorous acid solution 0.1-0.5 parts, phosphorus pentoxide 5-15 parts, 35% hydrogenperoxide steam generator 0.1-0.5 parts, deionization
Water 0.1-2 parts, described isomeric alcohol polyethenoxy ether class compound has following formula R1O—(C2H4O)n—R2, wherein R1
For C10Or C13Any one isomery alkyl, R2For hydrogen atom or organic residue, n is EO numbers, described isomery alcohol polyoxy
Ethene ether compound EO numbers are any one of 2-3,5-6,8-10,12 and 15.
Further, it is made up of the component of following mass fraction：Isomeric alcohol polyethenoxy ether class compound 88-92 parts, 50%
Hypophosphorous acid solution 0.2-0.4 parts, phosphorus pentoxide 8-12 parts, 35% hydrogenperoxide steam generator 0.2-0.4 parts, deionized water 0.5-1.5
Part.
Further, it is made up of the component of following mass fraction：90 parts, 50% time of isomeric alcohol polyethenoxy ether class compound
0.2 part of phosphoric acid solution, 10 parts of phosphorus pentoxide, 0.35 part of 35% hydrogenperoxide steam generator, 0.55 part of deionized water.
A kind of preparation method of phosphate emulsifying agent, comprises the following steps：
1）Add isomeric alcohol polyethenoxy ether class compound in a kettle. first, and set mixer rotating speed as 50-
200rpm；
2）After again in use reactor is heated to 45-70 DEG C, 30min is incubated；
3）After temperature of reaction kettle decreases below 45 DEG C, 50% hypophosphorous acid solution is added, after the completion of addition and mix 10-
60min；
4）Using dropper be added dropwise phosphorus pentoxide, and during dropwise addition control temperature of reaction kettle between 45-70 DEG C；
5）After phosphorus pentoxide is added dropwise to complete, 0.5-3h is incubated；
6）Reactor heating is given, and is heated to 70-110 DEG C, insulation 1-1.5h；
7）Deionized water is added, and is maintained the temperature between 70-110 DEG C, be incubated 1-1.5h；
8）After question response kettle temperature degree is cooled to 45-70 DEG C, 35% hydrogenperoxide steam generator is added to mix 10-50min；
9）Product is taken out and first passes through 1 m PP membrane filtrations, then filtered by 300 mesh stainless steel filters, obtain final products.
Further, step 4）Used in dropper be added dropwise phosphorus pentoxide speed be 2s/ drops.
Beneficial effect：
1. cost of material of the present invention is low, relatively cheap.
2. the present invention is of many uses, does not contain formaldehyde, safety and environmental protection.
3. good stability of the present invention, emulsifying effectiveness is good, it is emulsified after agent particle size it is less, be more evenly distributed, after emulsification
Gel is less.
Present invention improves the corrosion resistance of macromolecule membrane, heat endurance and photostability.
Specific embodiment
In conjunction with the embodiments, the present invention is described in further details.
Isomeric alcohol polyethenoxy ether class compound source model FANSAMAX TDA-20, the TDA- being related in the present invention
30th, TDA-50, TDA-60, TDA-80, TDA-90, TDA-100, IDA-50, IDA-90 and RHODASURF BC-720, BC-
610th, BC-690, BC-840 series and Exxon Mobil E-1302, E-1306, E-1308, E-1309, E-1310, E-1312,
Any one in SF-90 is used as raw material.
Embodiment one：A kind of phosphate emulsifying agent, is made up of the component of following mass fraction：Isomeric alcohol polyethenoxy ether class
91 parts of compound, 0.2 part of 50% hypophosphorous acid solution, 8.5 parts of phosphorus pentoxide, 0.35 part of 35% hydrogenperoxide steam generator, deionized water
0.2 part.
The isomeric alcohol polyethenoxy ether class compound has following formula R1O—(C2H4O)n—R2, wherein R1For C13
A kind of isomery alkyl, R2For hydrogen atom or organic residue, n is EO numbers, described isomeric alcohol polyethenoxy ether class compound
Take the RHODASURF BC-690 of EO numbers 9.
A kind of preparation method of phosphate emulsifying agent, comprises the following steps：
1）Add isomeric alcohol polyethenoxy ether class compound in a kettle. first, and set mixer rotating speed as 50rpm；
2）After again in use reactor is heated to 55 DEG C, 30min is incubated；
3）After temperature of reaction kettle decreases below 45 DEG C, 50% hypophosphorous acid solution is added, after the completion of addition and mixed
20min；
4）Phosphorus pentoxide is added dropwise using dropper, the speed that phosphorus pentoxide is added dropwise is 2s/ drops, and is controlled during dropwise addition
Temperature of reaction kettle is between 45-70 DEG C；
5）After phosphorus pentoxide is added dropwise to complete, 1h is incubated；
6）Reactor heating is given, and is heated to 80 DEG C, insulation 1h；
7）Deionized water is added, and is maintained the temperature between 70-110 DEG C, be incubated 1h；
8）After question response kettle temperature degree is cooled to 55 DEG C, 35% hydrogenperoxide steam generator is added to mix 20min；
9）Product is taken out and first passes through 1 m PP membrane filtrations, then filtered by 300 mesh stainless steel filters, obtain final products.
The index of final products be at 25 DEG C outward appearance be micro- turbid thick liquid, maximum moisture content 0.8%, maximum nonionic
Content of material 18%, color and luster is less than 2.0 Gardner, acid number 62.0-68.0 mgKOH/g, surface tension 32-42 mN/m.
Embodiment two：A kind of phosphate emulsifying agent, is made up of the component of following mass fraction：Isomeric alcohol polyethenoxy ether class
88 parts of compound, 0.2 part of 50% hypophosphorous acid solution, 11 parts of phosphorus pentoxide, 0.2 part of 35% hydrogenperoxide steam generator, deionized water 0.5
Part.
The isomeric alcohol polyethenoxy ether class compound has following formula R1O—(C2H4O)n—R2, wherein R1For C13
A kind of isomery alkyl, R2For hydrogen atom or organic residue, n is EO numbers, described isomeric alcohol polyethenoxy ether class compound
Take the FANSAMAX IDA-70 of EO numbers 7.
A kind of preparation method of phosphate emulsifying agent, comprises the following steps：
1）Add isomeric alcohol polyethenoxy ether class compound in a kettle. first, and set mixer rotating speed as 100rpm；
2）After again in use reactor is heated to 60 DEG C, 30min is incubated；
3）After temperature of reaction kettle decreases below 45 DEG C, 50% hypophosphorous acid solution is added, after the completion of addition and mixed
30min；
4）Phosphorus pentoxide is added dropwise using dropper, the speed that phosphorus pentoxide is added dropwise is 2s/ drops, and is controlled during dropwise addition
Temperature of reaction kettle is between 45-70 DEG C；
5）After phosphorus pentoxide is added dropwise to complete, 2h is incubated；
6）Reactor heating is given, and is heated to 90 DEG C, insulation 1.5h；
7）Deionized water is added, and is maintained the temperature between 70-110 DEG C, be incubated 1h；
8）After question response kettle temperature degree is cooled to 60 DEG C, 35% hydrogenperoxide steam generator is added to mix 30min；
9）Product is taken out and first passes through 1 m PP membrane filtrations, then filtered by 300 mesh stainless steel filters, obtain final products.
The index of final products be at 25 DEG C outward appearance be micro- turbid thick liquid, maximum moisture content 0.8%, maximum nonionic
Content of material 10%, color and luster is less than 2.0 Gardner, acid number 75.0-85.0 mgKOH/g, surface tension 30-40 mN/m.
Embodiment three：A kind of phosphate emulsifying agent, is made up of the component of following mass fraction：Isomeric alcohol polyethenoxy ether class
90 parts of compound, 0.2 part of 50% hypophosphorous acid solution, 9 parts of phosphorus pentoxide, 0.25 part of 35% hydrogenperoxide steam generator, deionized water 0.4
Part.
The isomeric alcohol polyethenoxy ether class compound has following formula R1O—(C2H4O)n—R2, wherein R1For C10
A kind of isomery alkyl, R2For hydrogen atom or organic residue, n is EO numbers, described isomeric alcohol polyethenoxy ether class compound
Take the Exxon Mobil SF-90 of EO numbers 9.
A kind of preparation method of phosphate emulsifying agent, comprises the following steps：
1）Add isomeric alcohol polyethenoxy ether class compound in a kettle. first, and set mixer rotating speed as 150rpm；
2）After again in use reactor is heated to 65 DEG C, 30min is incubated；
3）After temperature of reaction kettle decreases below 45 DEG C, 50% hypophosphorous acid solution is added, after the completion of addition and mixed
50min；
4）Phosphorus pentoxide is added dropwise using dropper, the speed that phosphorus pentoxide is added dropwise is 2s/ drops, and is controlled during dropwise addition
Temperature of reaction kettle is between 45-70 DEG C；
5）After phosphorus pentoxide is added dropwise to complete, 2.5h is incubated；
6）Reactor heating is given, and is heated to 100 DEG C, insulation 1h；
7）Deionized water is added, and is maintained the temperature between 70-110 DEG C, be incubated 1.5h；
8）After question response kettle temperature degree is cooled to 65 DEG C, 35% hydrogenperoxide steam generator is added to mix 40min；
9）Product is taken out and first passes through 1 m PP membrane filtrations, then filtered by 300 mesh stainless steel filters, obtain final products.
The index of final products be at 25 DEG C outward appearance be micro- turbid thick liquid, maximum moisture content 0.8%, maximum nonionic
Content of material 10%, color and luster is less than 2.0 Gardner, acid number 65.0-75.0 mgKOH/g, surface tension 30-40 mN/m.
The general principle and principal character and advantages of the present invention of the present invention, the technology of the industry has been shown and described above
Personnel it should be appreciated that the present invention is not restricted to the described embodiments, the simply explanation described in above-described embodiment and specification this
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, these changes
Change and improvement is both fallen within scope of the claimed invention, invention is claimed, and scope is by appending claims and its waits
Effect thing is defined.
Claims (5)
1. a kind of phosphate emulsifying agent, it is characterised in that be made up of the component of following mass fraction：Isomeric alcohol polyethenoxy ether class
Compound 85-95 parts, 50% hypophosphorous acid solution 0.1-0.5 parts, phosphorus pentoxide 5-15 parts, 35% hydrogenperoxide steam generator 0.1-0.5
Part, deionized water 0.1-2 part, described isomeric alcohol polyethenoxy ether class compound has following formula R1O—(C2H4O)n—
R2, wherein R1 is C10Or C13Any one isomery alkyl, R2For hydrogen atom or organic residue, n is EO numbers, and described is different
Structure alcohol polyethenoxy ether class compound EO numbers are any one of 2-3,5-6,8-10,12 and 15.
2. a kind of phosphate emulsifying agent according to claim 1, it is characterised in that by the component group of following mass fraction
Into：Isomeric alcohol polyethenoxy ether class compound 88-92 parts, 50% hypophosphorous acid solution 0.2-0.4 parts, phosphorus pentoxide 8-12 parts,
35% hydrogenperoxide steam generator 0.2-0.4 parts, deionized water 0.5-1.5 part.
3. a kind of phosphate emulsifying agent according to claim 1, it is characterised in that by the component group of following mass fraction
Into：90 parts of isomeric alcohol polyethenoxy ether class compound, 0.2 part of 50% hypophosphorous acid solution, 10 parts of phosphorus pentoxide, 35% hydrogen peroxide
0.35 part of solution, 0.55 part of deionized water.
4. a kind of preparation method of phosphate emulsifying agent, it is characterised in that comprise the following steps：
1) add isomeric alcohol polyethenoxy ether class compound in a kettle. first, and set mixer rotating speed as 50-200rpm；
2) after again in use reactor is heated to 45-70 DEG C, it is incubated 30min；
3) after temperature of reaction kettle decreases below 45 DEG C, 50% hypophosphorous acid solution is added, after the completion of addition and mixes 10-
60min；
4) using dropper be added dropwise phosphorus pentoxide, and during dropwise addition control temperature of reaction kettle between 45-70 DEG C；
5) after phosphorus pentoxide is added dropwise to complete, it is incubated 0.5-3h；
6) heat to reactor, and be heated to 70-110 DEG C, insulation 1-1.5h；
7) deionized water is added, and is maintained the temperature between 70-110 DEG C, be incubated 1-1.5h；
8) after question response kettle temperature degree is cooled to 45-70 DEG C, 35% hydrogenperoxide steam generator is added to mix 10-50min；
9) product is taken out and first passes through 1 m PP membrane filtrations, then filtered by 300 mesh stainless steel filters, obtain final products.
5. a kind of preparation method of phosphate emulsifying agent according to claim 4, it is characterised in that step 4）Used in drip
It is 2s/ drops that pipe is added dropwise the speed of phosphorus pentoxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201611133213.7A CN106632739A (en) | 2016-12-10 | 2016-12-10 | Phosphate emulsifier and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611133213.7A CN106632739A (en) | 2016-12-10 | 2016-12-10 | Phosphate emulsifier and preparation method thereof |
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| CN201611133213.7A Pending CN106632739A (en) | 2016-12-10 | 2016-12-10 | Phosphate emulsifier and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112424295A (en) * | 2018-06-27 | 2021-02-26 | 陶氏环球技术有限责任公司 | Phosphate surfactant compositions |
| CN114874784A (en) * | 2022-03-17 | 2022-08-09 | 上海保立佳新材料有限公司 | Isoalcohol polyoxyethylene ether phosphate ester emulsifier and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112424295A (en) * | 2018-06-27 | 2021-02-26 | 陶氏环球技术有限责任公司 | Phosphate surfactant compositions |
| US20210253869A1 (en) * | 2018-06-27 | 2021-08-19 | Dow Global Technologies Llc | Phosphate surfactant compositions |
| US11584857B2 (en) * | 2018-06-27 | 2023-02-21 | Dow Global Technologies Llc | Phosphate surfactant compositions |
| CN112424295B (en) * | 2018-06-27 | 2024-01-26 | 陶氏环球技术有限责任公司 | Phosphate surfactant composition |
| CN114874784A (en) * | 2022-03-17 | 2022-08-09 | 上海保立佳新材料有限公司 | Isoalcohol polyoxyethylene ether phosphate ester emulsifier and preparation method thereof |
| WO2023173535A1 (en) * | 2022-03-17 | 2023-09-21 | 上海保立佳新材料有限公司 | Isomeric alcohol polyoxyethylene ether phosphoric ester salt emulsifier and preparation method therefor |
| CN114874784B (en) * | 2022-03-17 | 2024-02-13 | 上海保立佳新材料有限公司 | Isomeric alcohol polyoxyethylene ether phosphate ester emulsifier and preparation method thereof |
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Application publication date: 20170510 |