CN104119226A - Synthetic method of novel adipate cold-resistant plasticizing agent - Google Patents
Synthetic method of novel adipate cold-resistant plasticizing agent Download PDFInfo
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- CN104119226A CN104119226A CN201410291254.3A CN201410291254A CN104119226A CN 104119226 A CN104119226 A CN 104119226A CN 201410291254 A CN201410291254 A CN 201410291254A CN 104119226 A CN104119226 A CN 104119226A
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- alcohol
- synthetic method
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- adipic acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the field of synthesis of chemicals and particularly relates to a synthetic method of a novel adipate cold-resistant plasticizing agent. The synthetic method comprises the following steps of: (1) adding alcohol and adipic acid which is 25%-40% of the weight of the alcohol to a reaction kettle, then adding sulfuric acid which is 0.1%-0.5% of the total weight and active carbon which is 0.1%-0.3% of the total weight, controlling heating speed in vacuum, and reacting at 120-150 DEG C for 1-5 hours; (2) after the reaction is finished, neutralizing, washing with water, and finally carrying out dehydration and pressure filtration to obtain a finished product, wherein the alcohol added to the reaction kettle in the step (1) can be decanol, isononyl alcohol or 810 alcohol. According to the synthetic method, 2-ethylhexanol in adipic acid (2-ethyl) hexyl is substituted with higher-class alcohol, so that the molecular weight is increased, the molecular chain length of a product is lengthened, and the product has better volatility resistance, extraction resistance and transfer resistance when used in a PVC (Polyvinyl Chloride) product.
Description
Technical field
The invention belongs to the synthetic field of chemical substance, relate in particular to a kind of synthetic method of novel adipic acid ester class cold resistant plasticizer.
Background technology
The own ester of softening agent hexanodioic acid (2-ethyl) is that DOA is a kind of cold resistant plasticizer of generally using, but its molecular chain is shorter, and molecular weight, so it is poor to use the volatility resistance in PVC goods, resistance to extractable and resistance to migration.
Summary of the invention
Defect and deficiency that the present invention exists in order to solve above-mentioned prior art, provide a kind of and can improve molecular weight, increase molecular chain length, make the synthetic method of the better novel adipic acid ester class cold resistant plasticizer of its volatility resistance for PVC goods, resistance to extractable and resistance to migration.
Technical scheme of the present invention: a kind of synthetic method of novel adipic acid ester class cold resistant plasticizer, comprises the steps:
1) in reactor, drop into the hexanodioic acid of alcohol and quality 25-40% thereof, then add the sulfuric acid of total mass 0.1%-0.5% and the gac of 0.1-0.3%; Under vacuum, control rate of warming, at 120-150 ℃, react 1-5 hour;
2) reaction finishes rear neutralization washing, and the press filtration of finally dewatering obtains finished product.
Step 1) alcohol dropping in reactor in can be a kind of in decyl alcohol, isononyl alcohol or 810 alcohol.
Preferably, step 1) the epoxy reaction still adopting in is three mouthfuls of beakers, step 1) in the alcohol that drops in reactor be decyl alcohol.
Preferably, in there-necked flask, drop into 400g decyl alcohol and 120g hexanodioic acid, then add 1.2 grams of sulfuric acid and 0.5 gram of gac, under vacuum, control rate of warming, at 120-150 ℃, react 1 hour, vacuum is removed in reaction end, after then neutralization washing, dehydration, obtains finished product.
Preferably, in there-necked flask, drop into 358g decyl alcohol and 120g hexanodioic acid, then add 1.2 grams of sulfuric acid and 0.5 gram of gac, under vacuum, control rate of warming, at 120-150 ℃, react 1 hour, vacuum is removed in reaction end, after then neutralization washing, dehydration, obtains finished product.
Preferably, in there-necked flask, drop into 400g decyl alcohol and 120g hexanodioic acid, then add 1.1 grams of sulfuric acid and 0.5 gram of gac, under vacuum, control rate of warming, at 120-150 ℃, react 1 hour, vacuum is removed in reaction end, after then neutralization washing, dehydration, obtains finished product.
Reaction equation of the present invention is: HOOC (CH
2)
4cOOH+2ROH=ROOC (CH
2)
4cOOR+2H
2o; Wherein R can be
in a kind of.
The present invention replaces the 2-Ethylhexyl Alcohol in the own ester of hexanodioic acid (2-ethyl) with more senior alcohol, improved molecular weight, has increased the molecular chain length of product, makes this product better for the volatility resistance of PVC goods, resistance to extractable and resistance to migration.
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, drop into 400g decyl alcohol and 120g hexanodioic acid, then add 1.2 grams of sulfuric acid and 0.5 gram of gac, under vacuum, control rate of warming, react 1 hour at 120-150 ℃, vacuum is removed in reaction end, after then neutralization washing, dehydration, obtains finished product.
Embodiment 2
In there-necked flask, drop into 358g decyl alcohol and 120g hexanodioic acid, then add 1.2 grams of sulfuric acid and 0.5 gram of gac, under vacuum, control rate of warming, react 1 hour at 120-150 ℃, vacuum is removed in reaction end, after then neutralization washing, dehydration, obtains finished product.
Embodiment 3HOOC (CH
2)
4cOOH+2ROH=ROOC (CH
2)
4cOOR+2H
2o
In there-necked flask, drop into 400g decyl alcohol and 120g hexanodioic acid, then add 1.1 grams of sulfuric acid and 0.5 gram of gac, under vacuum, control rate of warming, react 1 hour at 120-150 ℃, vacuum is removed in reaction end, after then neutralization washing, dehydration, obtains finished product.
The made product parameters of 3 embodiment of the present invention is as following table:
Claims (5)
1. a synthetic method for novel adipic acid ester class cold resistant plasticizer, is characterized in that: it comprises the steps:
1) in reactor, drop into the hexanodioic acid of alcohol and quality 25-40% thereof, then add the sulfuric acid of total mass 0.1%-0.5% and the gac of 0.1-0.3%; Under vacuum, control rate of warming, at 120-150 ℃, react 1-5 hour;
2) reaction finishes rear neutralization washing, and the press filtration of finally dewatering obtains finished product.
Step 1) alcohol dropping in reactor in can be a kind of in decyl alcohol, isononyl alcohol or 810 alcohol.
2. the synthetic method of a kind of novel adipic acid ester class cold resistant plasticizer according to claim 1, is characterized in that: step 1) in the reactor that adopts be three mouthfuls of beakers, step 1) in the alcohol that drops in reactor be decyl alcohol.
3. the synthetic method of a kind of novel adipic acid ester class cold resistant plasticizer according to claim 2, it is characterized in that: in there-necked flask, drop into 400g decyl alcohol and 120g hexanodioic acid, add again 1.2 grams of sulfuric acid and 0.5 gram of gac, under vacuum, control rate of warming, at 120-150 ℃, react 1 hour, vacuum is removed in reaction end, after then neutralization washing, dehydration, obtains finished product.
4. the synthetic method of a kind of novel adipic acid ester class cold resistant plasticizer according to claim 2, it is characterized in that: in there-necked flask, drop into 358g decyl alcohol and 120g hexanodioic acid, add again 1.2 grams of sulfuric acid and 0.5 gram of gac, under vacuum, control rate of warming, at 120-150 ℃, react 1 hour, vacuum is removed in reaction end, after then neutralization washing, dehydration, obtains finished product.
5. the synthetic method of a kind of novel adipic acid ester class cold resistant plasticizer according to claim 2, it is characterized in that: in there-necked flask, drop into 400g decyl alcohol and 120g hexanodioic acid, add again 1.1 grams of sulfuric acid and 0.5 gram of gac, under vacuum, control rate of warming, at 120-150 ℃, react 1 hour, vacuum is removed in reaction end, after then neutralization washing, dehydration, obtains finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410291254.3A CN104119226A (en) | 2014-06-25 | 2014-06-25 | Synthetic method of novel adipate cold-resistant plasticizing agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410291254.3A CN104119226A (en) | 2014-06-25 | 2014-06-25 | Synthetic method of novel adipate cold-resistant plasticizing agent |
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| CN104119226A true CN104119226A (en) | 2014-10-29 |
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ID=51764896
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| CN201410291254.3A Pending CN104119226A (en) | 2014-06-25 | 2014-06-25 | Synthetic method of novel adipate cold-resistant plasticizing agent |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104961924A (en) * | 2015-06-18 | 2015-10-07 | 张家港市大能塑料制品有限公司 | Cold-resistant plasticizer |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102226013A (en) * | 2011-05-05 | 2011-10-26 | 浙江建业化工股份有限公司 | Method for producing cold-resistant plasticizer through by-product nylon acids |
| CN102766046A (en) * | 2012-08-15 | 2012-11-07 | 淄博轩翌化工有限公司 | Method for preparing environment-friendly plasticizer diisodecyl adipate (DIDA) |
| WO2014005932A1 (en) * | 2012-07-06 | 2014-01-09 | Basf Se | The use of carboxylic acid esters as lubricants |
| CN103664597A (en) * | 2013-11-27 | 2014-03-26 | 浙江海利业科技有限公司 | Novel synthesis technology of adipic acid (2-propyl heptyl) ester |
-
2014
- 2014-06-25 CN CN201410291254.3A patent/CN104119226A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102226013A (en) * | 2011-05-05 | 2011-10-26 | 浙江建业化工股份有限公司 | Method for producing cold-resistant plasticizer through by-product nylon acids |
| WO2014005932A1 (en) * | 2012-07-06 | 2014-01-09 | Basf Se | The use of carboxylic acid esters as lubricants |
| CN102766046A (en) * | 2012-08-15 | 2012-11-07 | 淄博轩翌化工有限公司 | Method for preparing environment-friendly plasticizer diisodecyl adipate (DIDA) |
| CN103664597A (en) * | 2013-11-27 | 2014-03-26 | 浙江海利业科技有限公司 | Novel synthesis technology of adipic acid (2-propyl heptyl) ester |
Non-Patent Citations (1)
| Title |
|---|
| 王树清等: "耐寒性增塑剂己二酸正辛正癸酯合成工艺研究", 《现代塑料加工应用》, vol. 16, no. 4, 20 August 2004 (2004-08-20) * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104961924A (en) * | 2015-06-18 | 2015-10-07 | 张家港市大能塑料制品有限公司 | Cold-resistant plasticizer |
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Application publication date: 20141029 |