CN1687201A - Method for preparing superfine nucleator in organic phosphate class - Google Patents
Method for preparing superfine nucleator in organic phosphate class Download PDFInfo
- Publication number
- CN1687201A CN1687201A CN 200510024982 CN200510024982A CN1687201A CN 1687201 A CN1687201 A CN 1687201A CN 200510024982 CN200510024982 CN 200510024982 CN 200510024982 A CN200510024982 A CN 200510024982A CN 1687201 A CN1687201 A CN 1687201A
- Authority
- CN
- China
- Prior art keywords
- nucleator
- organic phosphate
- phenyl
- tert
- butyl
- 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
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention discloses an ultrafine organic phosphate nucleating agent and its preparation method. Said method includes the following steps: dissolving organic phosphate nucleating agent in organic solvent, adding surfactant, under the action of stirring adding water to the above-mentioned solution, then collecting the described ultrafine organic phosphate nucleating agent from the reaction product. Its average particle size is less than 0.3 micrometer.
Description
Technical field
The present invention relates to a kind of preparation method of superfine nucleator in organic phosphate class.
Background technology
Therefore nucleator in organic phosphate class is widely used in the MODIFICATION OF POLYPROPYLENE owing to have nontoxic, odorlessness, heat resisting temperature advantages of higher.But because such nucleator fusing point is higher, insoluble molten under polyacrylic processing temperature, cause its dispersed relatively poor in polypropylene, thereby influenced nucleation efficient, cause usage quantity to increase, the cost rising is too big, thereby has limited its widespread use.Can improve its dispersiveness in polypropylene and reduce the nucleator particle diameter, thereby improve nucleation efficient.
Usually the preparation of superfine nucleator in organic phosphate class is the method that adopts mechanical disintegration.Zhu Weiping, Wang Yaming etc. have reported that in Chinese patent (CN1432594) adopting common pulverizing legal system to be equipped with median size is the metal alkylide phosphoric acid salt nucleator of 0.5～100um.But adopt the nucleator particle diameter of single breaking method preparation big, size distribution is wide.The Takahashi Masayuki of Japan rising sun electrification company and Haruna Tohru etc. have reported that in European patent (EP1209190) method that adopts ball milling to combine with jet mill prepares nucleator in organic phosphate class.They at first ground the nucleator crude product 0.5 hour in jet mill, and then grinding in ball grinder 2.5 hours, having obtained median size at last was the nucleator in organic phosphate class of 0.3um.Because this method need be ground raw material in two kinds of different equipment, and milling time is longer, thereby facility investment is big, energy expenditure is high, and output is not high.
Summary of the invention
The technical issues that need to address of the present invention are the preparation methods that disclose a kind of ultra-fine organic phosphate nucleating agent, to overcome the above-mentioned defective that prior art exists.
Technical conceive of the present invention is such:
With the nucleator in organic phosphate class dissolving crude product in organic solvent, add tensio-active agent, under the effect of stirring, add water then and make it to separate out,, thereby obtain superfine nucleator in organic phosphate class because the existence of tensio-active agent can be controlled the particle diameter that nucleator is separated out effectively.
Technology of the present invention comprises the steps:
(1) with the dissolving crude product of nucleator in organic phosphate class in organic solvent, add tensio-active agent; The general structure of said nucleator in organic phosphate class crude product is as follows:
Wherein: R
1, R
2Represent C
1-C
12Alkyl, nitro, halogen, aryl;
R
3Represent C
1-C
4Alkyl, oxygen or sulphur;
M is basic metal or alkaline-earth metal, and preferred basic metal is for being lithium, sodium or potassium, and preferred alkaline-earth metal is calcium, magnesium or barium;
N is 1 or 2;
Said nucleator in organic phosphate class crude product can adopt the CN1358728 disclosed method to be prepared, or adopts the commercially available prod;
Preferred nucleator in organic phosphate class comprises 2,2 '-methylene radical-two (4, the 6-di-tert-butyl-phenyl) sodium phosphate, 2,2 '-methylene radical-two (4, the 6-di-tert-butyl-phenyl) Trilithium phosphate, 2,2 '-methylene radical-two (4, the 6-di-tert-butyl-phenyl) potassiumphosphate, 2,2 '-methylene radical-two (4 ,-di-tert-butyl-phenyl) calcium phosphate, 2,2 '-methylene radical-two (4, the 6-di-tert-butyl-phenyl) trimagnesium phosphate.
Said organic solvent is selected from a kind of or mixture in methyl alcohol, ethanol, propyl alcohol, sherwood oil, butanols, tetrahydrofuran (THF), dimethyl formamide or the acetone;
Said tensio-active agent is selected from a kind of or mixture in sodium lauryl sulphate, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, octadecyl trimethyl ammonium chloride, octadecyl trimethylammonium bromide, palmityl trimethyl ammonium chloride, cetyl trimethylammonium bromide, polyoxyethylene glycol or the fats Soxylat A 25-7;
Preferred polyoxyethylene octyl phenyl ether of said fats Soxylat A 25-7 or polyoxyethylene nonylplenyl ether;
The consumption of tensio-active agent is 0.01%～5% of a system gross weight, is preferably 0.1%～3%;
(2) under the effect of stirring, water is joined in the solution of step (1) gained, machine phosphoric acid salt nucleator is separated out, adopt ordinary method to collect said superfine nucleator in organic phosphate class then from the product of step (2), vertically median size is 0.1～0.3um;
Water is 1: 2～10: 1 with the volume of organic solvent ratio, is preferably 1: 1～4: 1;
Separating out temperature is 0 ℃～80 ℃, is preferably 10 ℃～40 ℃;
The time of separating out is 5min～120min, is preferably 10min～60min;
Technology of the present invention advantage compared with prior art is that output height, facility investment are few, province's energy.Because required equipment can utilize the suite of equipment of synthetic nucleator in organic phosphate class in this technology, thereby new installation need do not increased basically.Simultaneously because with respect to mechanical crushing equipment, the power of motor of reactor will be much smaller than the power of motor of mechanical crushing equipment, thereby can save the energy greatly.The present invention can obtain superfine nucleator in organic phosphate class easily, has the industrial applications prospect.
Embodiment
Embodiment 1
In the four-hole boiling flask that has agitator, thermometer, dropping funnel, reflux exchanger, add 20ml methyl alcohol, 5g2,2 '-methylene radical-two (4, the 6-di-tert-butyl-phenyl) sodium phosphate, the 0.6g polyoxyethylene octyl phenyl ether stirs, flask places 20 ℃ water bath with thermostatic control, drip 40ml water then, stir 30min, suction filtration, filter cake is dry 24hr under 80 ℃, obtains white powder 4.6g.Fusing point is greater than 400 ℃, yield 92%, vertically mean diameter 0.15um.
Embodiment 2
In the four-hole boiling flask that has agitator, thermometer, dropping funnel, reflux exchanger, add 20ml methyl alcohol, 5g2,2 '-methylene radical-two (4, the 6-di-tert-butyl-phenyl) sodium phosphate, the 0.6g sodium lauryl sulphate stirs, flask places 20 ℃ water bath with thermostatic control, drip 40ml water then, stir 30min, suction filtration, filter cake is dry 24hr under 80 ℃, obtains white powder 4.6g.Fusing point is greater than 400 ℃, yield 92%, vertically mean diameter 0.25um.
Embodiment 3
In the four-hole boiling flask that has agitator, thermometer, dropping funnel, reflux exchanger, add 20ml methyl alcohol, 5g2,2 '-methylene radical-two (4, the 6-di-tert-butyl-phenyl) calcium phosphate, the 0.6g polyoxyethylene octyl phenyl ether stirs, flask places 20 ℃ water bath with thermostatic control, drip 40ml water then, stir 30min, suction filtration, filter cake is dry 24hr under 80 ℃, obtains white powder 4.6g.Fusing point is greater than 400 ℃, yield 92%, vertically mean diameter 0.28um.
Claims (8)
1. the preparation method of a superfine nucleator in organic phosphate class is characterized in that, comprises the steps:
(1) with the dissolving crude product of nucleator in organic phosphate class in organic solvent, add tensio-active agent; The general structure of said nucleator in organic phosphate class crude product is as follows:
Wherein: R
1, R
2Represent C
1-C
12Alkyl, nitro, halogen, aryl;
R
3Represent C
1-C
4Alkyl, oxygen or sulphur;
M is basic metal or alkaline-earth metal, and n is 1 or 2;
(2) under the effect of stirring, water is joined in the solution of step (1) gained, machine phosphoric acid salt nucleator is separated out, adopt ordinary method from the product of step (2), to collect said superfine nucleator in organic phosphate class then.
2. method according to claim 1 is characterized in that, basic metal is lithium, sodium or potassium, and alkaline-earth metal is calcium, magnesium or barium.
3. method according to claim 1 is characterized in that, said organic solvent is selected from a kind of or mixture in methyl alcohol, ethanol, propyl alcohol, sherwood oil, butanols, tetrahydrofuran (THF), dimethyl formamide or the acetone.
4. method according to claim 1, it is characterized in that said tensio-active agent is selected from a kind of or mixture in sodium lauryl sulphate, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, octadecyl trimethyl ammonium chloride, octadecyl trimethylammonium bromide, palmityl trimethyl ammonium chloride, cetyl trimethylammonium bromide, polyoxyethylene glycol or the fats Soxylat A 25-7;
Said fats Soxylat A 25-7 is selected from polyoxyethylene octyl phenyl ether or polyoxyethylene nonylplenyl ether.
5. method according to claim 1 is characterized in that, the consumption of tensio-active agent is 0.01%～5% of a system gross weight.
6. method according to claim 1 is characterized in that, water is 1: 2～10: 1 with the volume of organic solvent ratio, and separating out temperature is 0 ℃～80 ℃, and the time of separating out is 5min～120min.
7. according to each described method of claim 1～5, it is characterized in that preferred nucleator in organic phosphate class comprises 2,2 '-methylene radical-two (4, the 6-di-tert-butyl-phenyl) sodium phosphate, 2,2 '-methylene radical-two (4, the 6-di-tert-butyl-phenyl) Trilithium phosphate, 2,2 '-methylene radical-two (4, the 6-di-tert-butyl-phenyl) potassiumphosphate, 2,2 '-methylene radical-two (4 ,-di-tert-butyl-phenyl) calcium phosphate, 2,2 '-methylene radical-two (4, the 6-di-tert-butyl-phenyl) trimagnesium phosphate.
8. method according to claim 7 is characterized in that, vertical median size of superfine nucleator in organic phosphate class is 0.1～0.3um.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510024982 CN1687201A (en) | 2005-04-08 | 2005-04-08 | Method for preparing superfine nucleator in organic phosphate class |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510024982 CN1687201A (en) | 2005-04-08 | 2005-04-08 | Method for preparing superfine nucleator in organic phosphate class |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1687201A true CN1687201A (en) | 2005-10-26 |
Family
ID=35305243
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510024982 Pending CN1687201A (en) | 2005-04-08 | 2005-04-08 | Method for preparing superfine nucleator in organic phosphate class |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1687201A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007096894A1 (en) * | 2006-02-27 | 2007-08-30 | Yissum Research Development Company Of The Hebrew University Of Jerusalem | Method for nucleating polymers |
| CN101665586B (en) * | 2008-09-05 | 2011-12-28 | 中国石油化工股份有限公司 | Method for preparing organic phosphate nucleating agent through ultrasonic sedimentation |
| CN102898724A (en) * | 2011-07-29 | 2013-01-30 | 中国石油化工股份有限公司 | Miniaturization amide type beta-polypropylene nucleating agent, preparation method thereof and polypropylene material |
| CN103788472A (en) * | 2012-10-30 | 2014-05-14 | 中国石油化工股份有限公司 | Binary composite polypropylene nucleating agent, preparation method and application |
| CN107849237A (en) * | 2015-07-22 | 2018-03-27 | 阿科玛法国公司 | The stable composition made of poly- (arylene ether ketone) (PAEK) in the molten state |
| CN109401060A (en) * | 2018-12-03 | 2019-03-01 | 四川大学 | The preparation method of aryl amide polypropylene beta nucleating agent |
-
2005
- 2005-04-08 CN CN 200510024982 patent/CN1687201A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007096894A1 (en) * | 2006-02-27 | 2007-08-30 | Yissum Research Development Company Of The Hebrew University Of Jerusalem | Method for nucleating polymers |
| CN101665586B (en) * | 2008-09-05 | 2011-12-28 | 中国石油化工股份有限公司 | Method for preparing organic phosphate nucleating agent through ultrasonic sedimentation |
| CN102898724A (en) * | 2011-07-29 | 2013-01-30 | 中国石油化工股份有限公司 | Miniaturization amide type beta-polypropylene nucleating agent, preparation method thereof and polypropylene material |
| CN102898724B (en) * | 2011-07-29 | 2014-11-05 | 中国石油化工股份有限公司 | Miniaturization amide type beta-polypropylene nucleating agent, preparation method thereof and polypropylene material |
| CN103788472A (en) * | 2012-10-30 | 2014-05-14 | 中国石油化工股份有限公司 | Binary composite polypropylene nucleating agent, preparation method and application |
| CN103788472B (en) * | 2012-10-30 | 2016-09-21 | 中国石油化工股份有限公司 | A kind of binary composite polypropylene nucleator, preparation method and application |
| CN107849237A (en) * | 2015-07-22 | 2018-03-27 | 阿科玛法国公司 | The stable composition made of poly- (arylene ether ketone) (PAEK) in the molten state |
| CN107849237B (en) * | 2015-07-22 | 2020-07-10 | 阿科玛法国公司 | Composition made of poly (arylene-ether-ketone) (PAEK) stable in the molten state |
| CN109401060A (en) * | 2018-12-03 | 2019-03-01 | 四川大学 | The preparation method of aryl amide polypropylene beta nucleating agent |
| CN109401060B (en) * | 2018-12-03 | 2020-07-31 | 四川大学 | Preparation method of aramid polyacrylamide β nucleating agent |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1687201A (en) | Method for preparing superfine nucleator in organic phosphate class | |
| CN102249255B (en) | Anionic-nonionic composite organic montmorillonite and preparation method thereof | |
| CN103724663B (en) | The preparation method of superfine active brucite composite modification material | |
| CN104592789A (en) | Method for preparing magnesium hydrate flame retardant | |
| CN101264893A (en) | Preparation method for bentonite | |
| CN109943099A (en) | A kind of fire retardant and preparation method thereof based on modified alpha zirconium phosphate | |
| CN101624516A (en) | Fluid loss additive of oil-base drilling fluid and preparation method thereof | |
| CN102977144A (en) | Organic hypophosphite containing triazine ring structure and method for preparing same | |
| CN103088460B (en) | A kind of High-strength industrial polyester fiber and preparation method thereof | |
| CN109264732A (en) | It is a kind of to have the function of reactivity preparation method for bentonite | |
| CN114806601B (en) | Alkyl phosphinate composition and preparation method and application thereof | |
| CN104559237A (en) | Non-ionic liquid crystal asphalt warm mixing agent and preparation method thereof | |
| CN102382034B (en) | Synthetic method of N-amino-3-azabicyclo[3,3,0]octane hydrochloride | |
| CN102775969B (en) | Multifunctional filtrate reducer and preparation method thereof | |
| CN101254927A (en) | Method for preparing active zinc borate by one-step proccess | |
| CN101450805B (en) | Novel process for synthesizing molecular sieve by calcining fly ash through wet alkalization | |
| CN112063016B (en) | Preparation method of long-acting phosphite ester antioxidant | |
| CN112111039B (en) | Dispersing agent, preparation method and application thereof | |
| CN103910370B (en) | A kind of ammonium salt dissolving and circulation ammonia process extract the method for aluminium hydroxide from flyash | |
| KR20120057189A (en) | Manufacturing methods of mineral solution and soil conditioner | |
| CN103787847B (en) | A kind of take ionic liquid as the technique of solvent continuous production trimethyl orthoacetate | |
| CN102259902A (en) | Superfine alpha-Al2O3 powder and preparation method thereof | |
| CN102382359B (en) | Preparation method of ultrafine organic phosphate nucleating agent | |
| CN106379921B (en) | A kind of method that industrial level lithium carbonate and battery-level lithium carbonate are produced using lithium phosphate waste material as raw material | |
| CN101423624A (en) | Miniaturization organic phoshate nucleating agent and preparation method thereof |
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 |
Open date: 20051026 |