CN104109258A - Synthetic method of high performance epoxy plasticizer - Google Patents
Synthetic method of high performance epoxy plasticizer Download PDFInfo
- Publication number
- CN104109258A CN104109258A CN201410293245.8A CN201410293245A CN104109258A CN 104109258 A CN104109258 A CN 104109258A CN 201410293245 A CN201410293245 A CN 201410293245A CN 104109258 A CN104109258 A CN 104109258A
- Authority
- CN
- China
- Prior art keywords
- grams
- reaction
- synthetic method
- hydrogen peroxide
- epoxy
- 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
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a synthetic method of a high performance epoxy plasticizer, which comprises the following steps: 1)adding vegetable fat and formic acid with 5-15% of mass of the vegetable fat in an epoxy reaction kettle, heating to the temperature of 40-80 DEG C; 2)adding hydrogen peroxide drop by drop with a catalyst having concentration of 30-50% while stirring, controlling the dropping speed, simultaneously cooling the material, controlling the reaction temperature of the material at 40-85 DEG C, continuously stirring for reaction for 2-10 hours after dropping is completed; and 3)separating water of the crude product by using a centrifuge and then neutralizing, then performing pressure reduction and dehydrating in a dehydration kettle. According to the invention, improvement of the production technology is carried out by using new catalyst and reasonable adjustment of the reaction condition, thereby side effect generated during the epoxy process is reduced, and the purpose for increasing stability and resistivity of epoxide group can be reached.
Description
Technical field
The invention belongs to the synthetic field of chemical substance, relate in particular to a kind of synthetic method of high-performance epoxy plasticizer.
Background technology
Epoxy plasticiser has satisfactory stability effect to light and heat, have high temperature resistant, low temperature resistant, do not move, the advantage such as no blooming, especially can produce good synergistic effect with the composite use of phthalate plasticizers.It can absorb the HCl that polyvinyl chloride resin is emitted in the time decomposing, again can be compatible with polyvinyl chloride resin, almost can, for all PVC goods, can obviously improve light stability and the thermostability of PVC goods.
The PVC plastics that use epoxy plasticiser, not only material cost can decrease, and its physical properties also has raising (as resistance to processibility, heat-resistant aging, folding resistance) in various degree.In the processing of soft, hard PVC goods, add corresponding epoxy soybean oil, can make the nontoxic goods of PVC, as the transparent article of PVC (clear vial, transparent box, food, drug packages material, medical product " transfusion bags ") etc.Equally, all to use epoxy plasticizer as the PVC plastics (as waterproof roll, plastic door-window, wallpaper plastic film) of open air use, to guarantee the premium propertiess such as goods are nontoxic, transparent.
Thereby the stability of epoxy plasticizer is more high better, but at present, in the manufacture method of epoxy plasticizer, the general sulfuric acid that adopts makees catalyzer, make it in epoxy process, can produce a series of unnecessary side reactions, thereby make the epoxy plasticizer epoxy retention rate resistivity of production all lower, can affect the stability of epoxy plasticizer.
Summary of the invention
Defect and deficiency that the present invention exists in order to solve above-mentioned prior art, provide a kind of by using new catalyzer and rationally adjusting reaction conditions production technique is improved, thereby reduce the side reaction producing in epoxy process, reached the synthetic method of the high-performance epoxy plasticizer of the object that improves epoxy group(ing) stability and resistivity.
Technical scheme of the present invention: a kind of synthetic method of high-performance epoxy plasticizer, comprises the steps:
1) in epoxy reaction still, add the formic acid of Vegetable oil lipoprotein and quality 5%-15% thereof, be warmed up to 40-80 DEG C;
2) stir the lower hydrogen peroxide that is added with catalyzer that concentration is 30%-50% that drips, control rate of addition, cooling material, makes the temperature of reaction of material be controlled at 40-85 DEG C simultaneously, after being added dropwise to complete, continues stirring reaction 2-10 hour;
3) divide water, neutralization by thick product with whizzer, then decompression dehydration in dehydrating kettle, finally filters, and obtains the nontoxic epoxy ester softening agent of environment-friendly type.
Preferably, step 1) in the epoxy reaction still that adopts be three mouthfuls of beakers, step 2) in the catalyzer that adds in hydrogen peroxide be phosphoric acid.
Preferably, in there-necked flask, adding quality is the vegetables oil of 165 grams, adding quality is the industrial formic acid of 9.6 grams again, be stirred and heated to 40 DEG C, after homo(io)thermism, drip 75 grams, 50% hydrogen peroxide that is mixed with catalyzer phosphoric acid, control temperature between 40-80 DEG C, continue reaction 10 hours, static layering, obtains finished product after neutralization washing, dewatering and filtering.
Preferably, in there-necked flask, adding quality is the vegetables oil of 165 grams, adding quality is the industrial formic acid of 8.4 grams again, be stirred and heated to 50 DEG C, after homo(io)thermism, drip 75 grams, 50% hydrogen peroxide that is mixed with catalyzer phosphoric acid, control temperature between 40-80 DEG C, continue reaction 10 hours, static layering, obtains finished product after neutralization washing, dewatering and filtering.
Preferably, in there-necked flask, adding quality is the vegetables oil of 165 grams, adding quality is the industrial formic acid of 8.4 grams again, be stirred and heated to 50 DEG C, after homo(io)thermism, drip 70 grams, 50% hydrogen peroxide that is mixed with catalyzer phosphoric acid, control temperature between 40-80 DEG C, continue reaction 10 hours, static layering, obtains finished product after neutralization washing, dewatering and filtering.
Reaction mechanism of the present invention is to comprise two reactions steps: 1. the preparation of peroxide agent: under the effect of catalyzer, hydrogen peroxide and formic acid effect generate peroxidation formic acid, and its reaction equation is:
2. the subacidity that this technology utilization hydrogen peroxide has, play at a certain temperature initiation, synthetic peroxide agent is reacted with Vegetable oil lipoprotein raw material, owing to mainly containing olein and linoleate in vegetables oil, they all have two keys in molecular structure, and peroxide agent is had an effect and generated corresponding epoxidation product with--C=C--key.And the peroxide phosphoric acid generating is played to stabilization, and ensureing that the Sauerstoffatom that peroxide phosphoric acid discharges can fully contact with the unsaturated link(age) in soybean oil, thereby epoxidation reaction is carried out to the direction of product, its reaction equation is:
Wherein R1 and R are substituting group, different and different according to the Vegetable oil lipoprotein kind of selecting.
The present invention is by using new catalyzer and rationally adjusting reaction conditions production technique is improved, thereby reduced the side reaction producing in epoxy process, reaches the object that improves epoxy group(ing) stability and resistivity.
Embodiment
Below in conjunction with embodiment, the present invention is further detailed explanation, but be not limiting the scope of the invention.
Embodiment 1
In there-necked flask, adding quality is the vegetables oil of 165 grams, adding quality is the industrial formic acid of 9.6 grams again, be stirred and heated to 40 DEG C, after homo(io)thermism, drip 75 grams, 50% hydrogen peroxide that is mixed with catalyzer phosphoric acid, control temperature between 40-80 DEG C, continue reaction 10 hours, static layering, obtains finished product after neutralization washing, dewatering and filtering.
Example 2
In there-necked flask, adding quality is the vegetables oil of 165 grams, adding quality is the industrial formic acid of 8.4 grams again, be stirred and heated to 50 DEG C, after homo(io)thermism, drip 75 grams, 50% hydrogen peroxide that is mixed with catalyzer phosphoric acid, control temperature between 40-80 DEG C, continue reaction 10 hours, static layering, obtains finished product after neutralization washing, dewatering and filtering.
Example 3
In there-necked flask, adding quality is the vegetables oil of 165 grams, adding quality is the industrial formic acid of 8.4 grams again, be stirred and heated to 50 DEG C, after homo(io)thermism, drip 70 grams, 50% hydrogen peroxide that is mixed with catalyzer phosphoric acid, control temperature between 40-80 DEG C, continue reaction 10 hours, static layering, obtains finished product after neutralization washing, dewatering and filtering.
The made product parameters of 3 embodiment of the present invention is as following table:
Claims (5)
1. a synthetic method for high-performance epoxy plasticizer, is characterized in that: it comprises the steps:
1) in epoxy reaction still, add the formic acid of Vegetable oil lipoprotein and quality 5%-15% thereof, be warmed up to 40-80 DEG C;
2) stir the lower hydrogen peroxide that is added with catalyzer that concentration is 30%-50% that drips, control rate of addition, cooling material, makes the temperature of reaction of material be controlled at 40-85 DEG C simultaneously, after being added dropwise to complete, continues stirring reaction 2-10 hour;
3) divide water, neutralization by thick product with whizzer, then decompression dehydration in dehydrating kettle, finally filters, and obtains the nontoxic epoxy ester softening agent of environment-friendly type.
2. the synthetic method of a kind of high-performance epoxy plasticizer according to claim 1, is characterized in that: step 1) in the epoxy reaction still that adopts be three mouthfuls of beakers, step 2) in the catalyzer that adds in hydrogen peroxide be phosphoric acid.
3. the synthetic method of a kind of high-performance epoxy plasticizer according to claim 2, it is characterized in that: in there-necked flask, adding quality is the vegetables oil of 165 grams, adding quality is the industrial formic acid of 9.6 grams again, be stirred and heated to 40 DEG C, after homo(io)thermism, drip 75 grams, 50% hydrogen peroxide that is mixed with catalyzer phosphoric acid, control temperature between 40-80 DEG C, continue reaction 10 hours, static layering, obtains finished product after neutralization washing, dewatering and filtering.
4. the synthetic method of a kind of high-performance epoxy plasticizer according to claim 2, it is characterized in that: in there-necked flask, adding quality is the vegetables oil of 165 grams, adding quality is the industrial formic acid of 8.4 grams again, be stirred and heated to 50 DEG C, after homo(io)thermism, drip 75 grams, 50% hydrogen peroxide that is mixed with catalyzer phosphoric acid, control temperature between 40-80 DEG C, continue reaction 10 hours, static layering, obtains finished product after neutralization washing, dewatering and filtering.
5. the synthetic method of a kind of high-performance epoxy plasticizer according to claim 2, it is characterized in that: in there-necked flask, adding quality is the vegetables oil of 165 grams, adding quality is the industrial formic acid of 8.4 grams again, be stirred and heated to 50 DEG C, after homo(io)thermism, drip 70 grams, 50% hydrogen peroxide that is mixed with catalyzer phosphoric acid, control temperature between 40-80 DEG C, continue reaction 10 hours, static layering, obtains finished product after neutralization washing, dewatering and filtering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410293245.8A CN104109258A (en) | 2014-06-25 | 2014-06-25 | Synthetic method of high performance epoxy plasticizer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410293245.8A CN104109258A (en) | 2014-06-25 | 2014-06-25 | Synthetic method of high performance epoxy plasticizer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104109258A true CN104109258A (en) | 2014-10-22 |
Family
ID=51706254
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410293245.8A Pending CN104109258A (en) | 2014-06-25 | 2014-06-25 | Synthetic method of high performance epoxy plasticizer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104109258A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105906586A (en) * | 2016-05-12 | 2016-08-31 | 中国林业科学研究院林产化学工业研究所 | Epoxy grease base plasticizing agent and preparation method thereof |
| CN106243744A (en) * | 2016-08-23 | 2016-12-21 | 成都米特瑞新材料科技有限公司 | Epoxy linseed oil improved plasticizer |
| CN110003808A (en) * | 2019-04-15 | 2019-07-12 | 四川卓邦安新材料科技有限公司 | A kind of high-polymer self-adhesion waterproof coiled material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1667106A (en) * | 2005-02-23 | 2005-09-14 | 华南理工大学 | Vegetable oil with high epoxy value and its preparing method and use |
| CN103113992A (en) * | 2013-01-21 | 2013-05-22 | 广州市新锦龙塑料助剂有限公司 | Method for selectively oxidizing and synthesizing epoxy cottonseed oil plasticizer by utilizing industrial coarse cottonseed oil |
-
2014
- 2014-06-25 CN CN201410293245.8A patent/CN104109258A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1667106A (en) * | 2005-02-23 | 2005-09-14 | 华南理工大学 | Vegetable oil with high epoxy value and its preparing method and use |
| CN103113992A (en) * | 2013-01-21 | 2013-05-22 | 广州市新锦龙塑料助剂有限公司 | Method for selectively oxidizing and synthesizing epoxy cottonseed oil plasticizer by utilizing industrial coarse cottonseed oil |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105906586A (en) * | 2016-05-12 | 2016-08-31 | 中国林业科学研究院林产化学工业研究所 | Epoxy grease base plasticizing agent and preparation method thereof |
| CN106243744A (en) * | 2016-08-23 | 2016-12-21 | 成都米特瑞新材料科技有限公司 | Epoxy linseed oil improved plasticizer |
| CN110003808A (en) * | 2019-04-15 | 2019-07-12 | 四川卓邦安新材料科技有限公司 | A kind of high-polymer self-adhesion waterproof coiled material and preparation method thereof |
| CN110003808B (en) * | 2019-04-15 | 2021-12-03 | 四川卓邦安新材料科技有限公司 | High-molecular self-adhesive waterproof coiled material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101570386B1 (en) | Composite plasticizer composition comprising epoxy ester compound and polymer resin composition using the same | |
| KR101981990B1 (en) | Plasticizer composition comprising naturally cardanol base plasticizer and vegetable oil base epoxidated, and polymer resin composition comprising the same | |
| CN107406621B (en) | Plasticizer composition, resin combination and preparation method thereof | |
| CN101691524A (en) | Method for preparing epoxidized soybean oil with high epoxy value by fractional step method | |
| CN108026322A (en) | Plasticizer composition and the resin combination comprising the plasticizer composition | |
| CN104109258A (en) | Synthetic method of high performance epoxy plasticizer | |
| CN102336981A (en) | Processing modifier for polyvinyl chloride plastic-wood material | |
| KR101454750B1 (en) | Improved process for preparing epoxidized fatty acid ester | |
| CN105566799A (en) | Environmental-protection type highly-transparent PVC composition for producing medical infusion tubes | |
| CN103666770B (en) | Preparation method of epoxy modified castor oil | |
| KR101899655B1 (en) | Plasticizer, resin composition and method for preparing them | |
| CN103524727A (en) | Preparation method of dibenzoate polyethylene glycol plasticizer | |
| CN102532748A (en) | Processing modifier for polyvinyl chloride electrical casing | |
| CN104004303B (en) | A kind of complex biological ester plasticizer | |
| CN106748774B (en) | Refining method of cyclohexane diformate plasticizer | |
| CN110804029B (en) | Epoxy plasticizer and preparation method thereof | |
| CN101613282A (en) | A kind of environment-friendly plasticizer cyclohexane alkane-1, the preparation method of 2-2-dicarboxylic acid diethylhexyl ester | |
| CN104529746B (en) | A kind of method of catalyst compounded synthesis of dimmer acid | |
| CN103755962A (en) | Production method for high-vinyl raw rubber | |
| CN105085883A (en) | Synthesis method of polyether ester plasticizer | |
| CN103936993A (en) | Method for preparing methyl silicone oil by utilizing sulfuric acid | |
| KR20160119695A (en) | Plasticizer, resin composition and method for preparing them | |
| CN102701980A (en) | Synthetic method of environmental-friendly plasticizer hexahydrobenzene diisononyl phthalate | |
| CN107857744A (en) | A kind of epoxy aliphatic acid methyl ester plasticizer production process and obtained plasticizer | |
| CN107641107A (en) | Diacetyl epoxy undecanoic acid glyceride and its preparation method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20141022 |