CN1084861A - A kind of igelite thermo-stabilizer and preparation thereof - Google Patents
A kind of igelite thermo-stabilizer and preparation thereof Download PDFInfo
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- CN1084861A CN1084861A CN 92111173 CN92111173A CN1084861A CN 1084861 A CN1084861 A CN 1084861A CN 92111173 CN92111173 CN 92111173 CN 92111173 A CN92111173 A CN 92111173A CN 1084861 A CN1084861 A CN 1084861A
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- stabilizer
- dibutyl tin
- tin laurate
- oxidation inhibitor
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Abstract
The present invention relates to a kind of igelite thermo-stabilizer and preparation technology thereof.This thermo-stabilizer is the collaborative mixture that is mixed with by dibutyl tin laurate and epoxy etc., is that polyvinyl chloride is soft, indispensable high effective additives in the boardy product processing.The PVC goods of being processed into through it have the transparency of height, and outstanding thermotolerance and weathering resistance, its performance are better than the pure product of dibutyl tin laurate, and it is cheap, are present ideal a kind of thermo-stabilizer kinds.
Description
The present invention relates to a kind of efficient thermo-stabilizer and preparation technology thereof who is used for polyvinyl chloride (being called for short " PVC ") plastic working, this invention belongs to the fine chemistry industry production field.
The thermo-stabilizer that the present invention mentions is one of organo-tin het stabilizer product innovation.This thermo-stabilizer is the collaborative mixture that is mixed with by dibutyl tin laurate (its chemical formula and structure are referring to accompanying drawing) and epoxy etc. (its commodity is called " capital tin C-102 ", below be called for short with this).Organo-tin het stabilizer is that polyvinyl chloride is soft, indispensable high effective additives in the boardy product processing, inserts the transparency and the outstanding characteristics such as thermotolerance that the polrvinyl chloride product of being processed into has height through it." capital tin C-102 " is mainly used in the processing of goods such as pearly-lustre that polyvinyl chloride resin makes or transparent plastics footwear, semi-rigid, transparent film, transparent hose, because and the synergistic effect between the each component makes its thermostability and excellent weather resistance and hard in the pure product of dibutyl tin laurate (it also is a kind of organo-tin het stabilizer kind commonly used), and can improve the whiteness of polyvinyl chloride resin.
The objective of the invention is to obtain PVC goods with extremely excellent weathering resistance, pearly-lustre, the transparency and compatibleness for the plastics industry that adapts to China's development different demands to stablizer." capital tin C-102 " no sulfide staining, no perviousness, its oilness is best in all organo-tin het stabilizers.Owing to the synergistic effect of these product and each component, make its thermostability.Anti-aging and ageing-resistant performance are better than other organotin stabilizer, are present ideal a kind of thermo-stabilizer kinds, and its price is lower than other organo-tin het stabilizer about 40%, so it is most widely used, prospect of production is very wide.
The processing method of the present invention's preparation " capital tin C-102 " is, with dibutyltin oxide and cocinic acid under normal pressure, in 50-90 ℃ of temperature range, carried out the oxidation building-up reactions 1-2 hour, obtain the dibutyl tin laurate crude product, make the pure product of dibutyl tin laurate, i.e. the present invention's " capital tin C-102 " main component through decompression dehydration, filtration two procedures then; Then under 50-90 ℃ of temperature, under agitation condition that quantitative dibutyl tin laurate, epoxy compounds, phenyl ester, sequestrant, oxidation inhibitor thorough mixing is even, promptly make " capital tin C-102 " thermo-stabilizer product.
Among the preparation technology of the present invention, used proportioning raw materials is: cocinic acid/dibutyltin oxide=1.5-2.5/1(weight ratio).
After the oxidation building-up reactions makes the dibutyl tin laurate crude product, carry out the decompression dehydration operation, required reduced pressure is for keeping vacuum tightness below 0.09MPa, and dehydration temperaturre is 70-120 ℃, and dewatering time control is as the criterion with the water that purifies in the crude product.
After obtaining the pure product of dibutyl tin laurate, in 50-90 ℃, under the 60-80 ℃ of temperature of being advisable, be mixed under agitation condition, its mixed ratio (weight ratio) is as follows:
Dibutyl tin laurate 35-70%
Epoxide 25-45%
Phenyl ester 5-20%
Sequestrant 0-3%
Oxidation inhibitor 0-3%
Wherein, dibutyl tin laurate is main component, and its best ratio range is 40-60%, epoxy compounds, i.e. epoxy plasticiser such as epoxy soybean oil or ethyl hexyl ester of epoxidized soybean oil; Phenyl ester, i.e. phthalic acid softening agent such as dioctyl phthalate (DOP); Sequestrant is as Phenyl Di-2-ethyl Hexyl Phosphite etc.; Oxidation inhibitor, [β (3 as four, the 5-di-tert-butyl-hydroxy phenyl) go through acid] tetramethylolmethane (being called for short " oxidation inhibitor KY-7910 ") or [β (3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] octadecanol ester oxidation inhibitor such as (being called for short " oxidation inhibitor KY-7920 ").
Advantage of the present invention just is:
(1) the present invention's processing soft for the PVC plastics, boardy product provides a kind of thermo-stabilizer of new and effective, low toxicity.
(2) the present invention has overcome the shortcoming of other thermo-stabilizer poor lubrication in plastic working, and the outward appearance of plastics is taken an evident turn for the better, and has improved the whiteness of polyvinyl chloride resin.
(3) because the present invention is a kind of by the formulated collaborative mixture of many kinds additives for plastics (softening agent, sequestrant, oxidation inhibitor and thermo-stabilizer), its suitability is strong, has made things convenient for the user, and is easy to use.
(4) product of the present invention, main component is self-produced, and other raw material also more cheaply is easy to get.
(5) preparation technology of the present invention, flow process is simple, process stabilizing, be easy to realize suitability for industrialized production.
Below further specify preparation technology of the present invention with embodiment, to help the understanding to the present invention and advantage thereof, but as to the qualification of protection domain of the present invention, it is decided by claim.
Embodiment 1:
At one vacuum system is housed, in the 500ml flask of condenser and agitator, accurately adds 172.9 gram cocinic acids, add 100 gram dibutyltin oxides subsequently, cover bottleneck completely, open stirring, stir and be warming up to 80 ℃, insulation was carried out the oxidation building-up reactions 1.5 hours.Reaction finishes to make the dibutyl tin laurate crude product.Open vacuum system subsequently, keep vacuum tightness below 0.09MPa, gradually the liquid temperature rise is caused 105 ℃, insulation, dehydration is 1 hour under this vacuum and temperature, and dehydration is finished postcooling and caused normal temperature, obtains pure product 260 grams of main component-dibutyl tin laurate of the present invention with the B suction filtration, these product are faint yellow, oily liquids, density (ρ
20 4) 1.084, refractive index (η
20 D) 1.4683.
In above-mentioned 500ml flask, add 260 gram dibutyl tin laurates, open stirring, be warming up to 75 ℃, insulation, accurately add 250 gram ethyl hexyl ester of epoxidized soybean oil, 45 gram dioctyl phthalate (DOP)s, 7 gram Phenyl Di-2-ethyl Hexyl Phosphites, 2 grams " oxidation inhibitor KY-7910 " then, be fully mixed to evenly, promptly make " capital tin C-102 " product.
Embodiment 2
At one vacuum system is housed, in the 500ml flask of condenser and agitator, accurately add 200.0 gram cocinic acids, 98.5 gram dibutyltin oxide, cover bottleneck completely, open stirring, stirring velocity is 140 rev/mins, be warming up to 65 ℃, insulation was carried out the oxidation building-up reactions 2 hours, reaction finishes to make the dibutyl tin laurate crude product, open vacuum system subsequently, keep below the vacuum tightness 0.09MPa, gradually with liquid temperature rise to 100 ℃, insulation, dehydration is 1.5 hours under this temperature and vacuum tightness, and dehydration is finished postcooling to normal temperature, obtains master's component-dibutyl tin laurate 282 grams of the present invention with the B suction filtration.These product are faint yellow, oily liquids, density (ρ
20 4) 1.084, refractive index (η
20 D) 1.468.
In above-mentioned 500ml flask, add 282 gram dibutyl tin laurates, open stirring, be warming up to 60 ℃, insulation adds 120 gram epoxy soybean oils, 70 gram dioctyl phthalate (DOP)s, 4 gram oxidation inhibitor KY-7920 then, is fully mixed to evenly promptly to make " capital tin C-102 " product.
Embodiment 3
Method by embodiment 1 makes pure product 260 grams of dibutyl tin laurate.
In the described 500ml flask of above-mentioned example, accurately add 260 gram dibutyl tin laurates, open stirring, be warming up to 70 ℃, insulation adds 180 gram ethyl hexyl ester of epoxidized soybean oil, 45 gram dioctyl phthalate (DOP)s then, be fully mixed to evenly, promptly obtain " capital tin C-102 " product.
Embodiment 4
Make pure product 282 grams of dibutyl tin laurate by embodiment 2 described methods.
In the described 500ml flask of above-mentioned example, accurately add 282 gram dibutyl tin laurates, open stirring, be warming up to 65 ℃, insulation, add 180 gram epoxy soybean oils, 60 gram dioctyl phthalate (DOP)s, diisooctyl phenyl phosphite 8 grams then, be fully mixed to evenly, promptly obtain " capital tin C-102 " product.
Claims (13)
1, a kind of efficient thermo-stabilizer that is used for the processing of polyvinyl chloride plastic material products, trade name is " capital tin C-102 ", it is characterized in that:
(1) this thermo-stabilizer is the collaborative mixture that is mixed with by principal constituent dibutyl tin laurate and epoxy compounds, phenyl ester, sequestrant and oxidation inhibitor,
(2) this collaborative mixture is composed as follows
Dibutyl tin laurate 35～70%
Epoxy compounds 25～45%
Phenyl ester 5～20%
Sequestrant 0～3%
Oxidation inhibitor 0～3%
2, the structure by the described principal constituent dibutyl tin laurate of claim 1 is
3, by the content of the described major constituent dibutyl tin laurate of claim 1 with 40～60% for the most suitable.
4, by the described epoxy compounds of claim 1, epoxy plasticisers such as finger ring oxygen soybean oil or ethyl hexyl ester of epoxidized soybean oil.
5, by the described phenyl ester of claim 1, refer to dioctyl phthalate (DOP) and other phthalic ester plasticizer.
6, by the described sequestrant of claim 1, refer to diisooctyl phenyl phosphite.
7, by the described oxidation inhibitor of claim 1, refer to oxidation inhibitor such as four (β (3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol esters or (β (3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid) octadecanol ester.
8, can not contain sequestrant and oxidation inhibitor by the described thermo-stabilizer mixture of claim 1.
9, can not contain sequestrant by the described thermo-stabilizer mixture of claim 1.
10, can not contain oxidation inhibitor by the described thermo-stabilizer mixture of claim 1.
11, a kind of method that is used to prepare the thermo-stabilizer described in the claim 1 is characterized in that
(1) under condition of normal pressure, under 50～90 ℃ of temperature,, obtain the dibutyl tin laurate crude product with dibutyltin oxide and cocinic acid oxidation building-up reactions 1～2 hour,
(2) with this crude product carrying out decompression dehydration under the condition that keeps below the vacuum tightness 0.09MPa and under 70～120 ℃ of temperature, purify the moisture in the crude product,
(3) the dibutyl tin laurate crude product behind the filter dehydration obtains pure product,
(4) under 50～90 ℃ of temperature, under agitation condition that major constituent dibutyl tin laurate and epoxy compounds, phenyl ester, sequestrant, oxidation inhibitor thorough mixing is even, promptly obtain product of the present invention " capital tin C-102 ".
12, be to be advisable with 1.6～2.0/1 in cocinic acid/dibutyltin oxide=1.5～2.5/1 by the described synthesis material weight proportion of claim 11.
13, be advisable with 60～80 ℃ by the described temperature that is mixed of claim 11.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92111173 CN1084861A (en) | 1992-09-29 | 1992-09-29 | A kind of igelite thermo-stabilizer and preparation thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92111173 CN1084861A (en) | 1992-09-29 | 1992-09-29 | A kind of igelite thermo-stabilizer and preparation thereof |
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| Publication Number | Publication Date |
|---|---|
| CN1084861A true CN1084861A (en) | 1994-04-06 |
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ID=4945199
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| Application Number | Title | Priority Date | Filing Date |
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| CN 92111173 Pending CN1084861A (en) | 1992-09-29 | 1992-09-29 | A kind of igelite thermo-stabilizer and preparation thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103992510A (en) * | 2014-05-09 | 2014-08-20 | 广州市联诺化工科技有限公司 | An efficient liquid composite organo-tin heat stabilizer and a preparing method thereof |
| CN104497036A (en) * | 2014-12-05 | 2015-04-08 | 长沙罗斯科技有限公司 | Preparation technique of dibutyl tin diacetate |
| CN106280076A (en) * | 2016-08-05 | 2017-01-04 | 衢州建华东旭助剂有限公司 | Itaconic acid methyl stannum stabilizer for plastics and production method |
| CN107163075A (en) * | 2017-07-24 | 2017-09-15 | 西北有色金属研究院 | A kind of synthetic method of dibutyl tin laurate |
-
1992
- 1992-09-29 CN CN 92111173 patent/CN1084861A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103992510A (en) * | 2014-05-09 | 2014-08-20 | 广州市联诺化工科技有限公司 | An efficient liquid composite organo-tin heat stabilizer and a preparing method thereof |
| CN104497036A (en) * | 2014-12-05 | 2015-04-08 | 长沙罗斯科技有限公司 | Preparation technique of dibutyl tin diacetate |
| CN106280076A (en) * | 2016-08-05 | 2017-01-04 | 衢州建华东旭助剂有限公司 | Itaconic acid methyl stannum stabilizer for plastics and production method |
| CN107163075A (en) * | 2017-07-24 | 2017-09-15 | 西北有色金属研究院 | A kind of synthetic method of dibutyl tin laurate |
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