CN115260583A - Liquid barium-zinc composite stabilizer and preparation method thereof - Google Patents
Liquid barium-zinc composite stabilizer and preparation method thereof Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
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- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
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- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
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Abstract
The invention belongs to a stabilizer for a PVC film, and discloses a liquid barium-zinc composite stabilizer and a preparation method thereof. The raw materials of the liquid barium-zinc composite stabilizer comprise 190-240 parts of oleic acid, 90-120 parts of diethylene glycol monobutyl ether, 25-40 parts of isooctanoic acid, 30-50 parts of p-tert-butylbenzoic acid, 15-20 parts of zinc oxide, 90-120 parts of barium hydroxide monohydrate, 25-40 parts of antioxidant and 140-180 parts of phosphite ester, and the preparation method comprises the following steps: preheating, pumping in oleic acid, diethylene glycol monobutyl ether, isooctanoic acid and white oil, gradually raising the temperature, sequentially adding benzoic acid, p-tert-butyl benzoic acid, zinc oxide and barium hydroxide monohydrate, raising the temperature twice, maintaining the temperature, correcting the white oil, finally adding an antioxidant, phosphite ester and white oil, stirring, returning the liquid, cooling, filter-pressing and barreling. The liquid barium-zinc composite stabilizer prepared by the invention has strong stability, good colorability and high transparency, and can meet the transparency requirement of a PVC film.
Description
Technical Field
The invention relates to the technical field of stabilizers for PVC films, and particularly relates to a liquid barium-zinc composite stabilizer and a preparation method thereof.
Background
Polyvinyl chloride (PVC), english called PVC for short, is very widely used. The product has wide application in building materials, industrial products, daily necessities, floor leathers, floor tiles, artificial leathers, pipes, wires and cables, packaging films, bottles, foaming materials, sealing materials, fibers and the like. However, since PVC has poor processing thermal stability at high temperature and is not easy to process, a thermal stabilizer must be added to maintain its properties during molding.
The liquid barium-zinc composite stabilizer has different compositions, different properties, excellent thermal and light stability, small initial colorability, good transparency and color stability, stronger stabilizing effect than solid composite soaps, so the dosage can be reduced, generally 2 to 3 parts, no dust poisoning occurs, the liquid barium-zinc composite stabilizer is completely dissolved in common plasticizers, has good dispersibility and small precipitation tendency, and can be almost used in all fields from semi-rigid products to plasticized PVC, including calendering, extrusion, injection extrusion blow molding, injection blow molding and plastisol processing.
However, the existing liquid barium-zinc composite stabilizer has unreasonable raw material proportion, and is difficult to meet the transparency requirement of a PVC film when being used for PVC film processing.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a liquid barium-zinc composite stabilizer and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows: the liquid barium-zinc composite stabilizer is characterized in that raw materials for preparing the liquid barium-zinc composite stabilizer comprise, by weight, 190-240 parts of oleic acid, 90-120 parts of diethylene glycol monobutyl ether, 25-40 parts of isooctanoic acid, 30-50 parts of p-tert-butylbenzoic acid, 15-20 parts of zinc oxide, 90-120 parts of barium hydroxide monohydrate, 25-40 parts of an antioxidant and 140-180 parts of phosphite ester.
Preferably, the oleic acid and isooctanoic acid are both polycarbonic organic acids, both of which contribute to thermal stability and lubricity during formulation.
Preferably, the diethylene glycol butyl ether is used as a diluent and plays a role in assisting the complete reaction of the metal oxide.
Preferably, the antioxidant is an antioxidant 1076, and the phosphite is a secondary antioxidant.
As a further improvement of the scheme, the raw material components also comprise white oil, and the white oil accounts for 285-340 parts by weight.
As a further improvement of the scheme, the raw material components also comprise benzoic acid, and the benzoic acid accounts for 18-30 parts by weight.
The preparation method of the liquid barium-zinc composite stabilizer is characterized by comprising the following steps:
(1) Preheating: introducing heat-conducting oil into a jacket of the reaction kettle, heating and preheating the reaction kettle, and starting a stirring mechanism in the reaction kettle;
(2) The raw materials are added for the first time: opening a vacuum pump, and pumping liquid raw materials of oleic acid, diethylene glycol butyl ether, isooctanoic acid and white oil;
(3) Heating, and sequentially adding the following raw materials for the second time and the third time: adding benzoic acid and p-tert-butyl benzoic acid when the temperature is increased to 35-45 ℃, and adding zinc oxide and barium hydroxide monohydrate when the temperature is increased to 55-65 ℃;
(4) Secondary heating and heat preservation: when the temperature is increased to 95-105 ℃, the conduction oil is closed, the temperature is kept for 30-40 minutes, and the composition in the reaction kettle is changed from white turbidity to clear transparency through an observation sight glass of the reaction kettle;
(5) Heating again and preserving heat: introducing heat conducting oil again to heat the reaction kettle, closing heating when the temperature is raised to 130-135 ℃, and continuing to preserve heat for 30-40 minutes when the temperature is raised to 135-140 ℃;
(6) And (3) correction: vacuumizing for 10-12 minutes, weighing the discharged water, and supplementing white oil to the part exceeding 35kg;
(7) Finally, feeding and stirring raw materials: adding an antioxidant, phosphite ester, white oil and the white oil supplemented in the step (6), and continuously stirring;
(8) Returning liquid and barreling: returning the liquid, cooling to 80-85 ℃, filtering and barreling after the filtrate is clear.
Preferably, the preheating in step (1) is to 90-120 ℃.
Preferably, the stirring time in step (7) is 30 to 35 minutes.
The beneficial effects of the invention are: in the liquid barium-zinc composite stabilizer provided by the invention, the isooctanoic acid and the oleic acid are multi-carbon organic acids, and can play a role in thermal stability and lubricity in preparation, so that the stability of a product is improved; diethylene glycol monobutyl ether is used as a diluent to play a role in assisting the complete reaction of metal oxide (zinc oxide), an antioxidant 1076 and phosphite ester are respectively used as an antioxidant and an auxiliary oxidant, p-tert-butyl benzoic acid is used as an organic synthesis intermediate, white oil is favorable for increasing the brightness of a product, and benzoic acid is used as a plasticizer. The liquid barium-zinc composite stabilizer prepared by the invention has strong stability, good colorability and high transparency, and can meet the transparency requirement of a PVC film.
Detailed Description
The present invention is described in detail below by way of examples to facilitate understanding of the present invention by those skilled in the art, and it is to be specifically noted that the examples are provided only for the purpose of further illustrating the present invention and are not to be construed as limiting the scope of the present invention.
Example 1
The liquid barium-zinc composite stabilizer is prepared from the following raw materials, by weight, 220 parts of oleic acid, 110 parts of diethylene glycol butyl ether, 307 parts of white oil, 35 parts of isooctanoic acid, 20 parts of benzoic acid, 45 parts of p-tert-butyl benzoic acid, 18 parts of zinc oxide, 100 parts of barium hydroxide monohydrate, 30 parts of an antioxidant, 150 parts of phosphite ester and 1076 as the antioxidant.
A preparation method of a liquid barium-zinc composite stabilizer comprises the following steps:
(1) Preheating: introducing heat conducting oil into a jacket of the reaction kettle, heating the reaction kettle to preheat to 100 ℃, and starting a stirring mechanism in the reaction kettle;
(2) The raw materials are added for the first time: starting a vacuum pump, and pumping 207 parts of liquid raw materials of oleic acid, diethylene glycol butyl ether, isooctanoic acid and white oil;
(3) Heating, and sequentially adding the following raw materials for the second time and the third time: adding benzoic acid and p-tert-butyl benzoic acid when the temperature is raised to 40 ℃, and adding zinc oxide and barium hydroxide monohydrate when the temperature is raised to 60 ℃;
(4) Secondary heating and heat preservation: when the temperature is raised to 100 ℃, the conduction oil is closed, the temperature is kept for 30 minutes, and the composition in the reaction kettle is changed from white turbidity to clear transparency through an observation sight glass of the reaction kettle;
(5) Heating again and preserving heat: introducing heat transfer oil again to heat the reaction kettle, turning off heating when the temperature is raised to 132 ℃, and continuing to preserve heat for 40 minutes when the temperature is raised to 138 ℃;
(6) And (3) correction: vacuumizing for 10 minutes, and weighing the discharged water, wherein the weight of the water is 35kg;
(7) And (3) finally adding and stirring the raw materials: adding 100 parts of antioxidant, phosphite ester and white oil, and continuously stirring for 30 minutes;
(8) Returning liquid and barreling: returning the liquid, cooling to 85 ℃, filtering the clear filtrate, and barreling.
Example 2
The liquid barium-zinc composite stabilizer is prepared from the following raw materials, by weight, 240 parts of oleic acid, 100 parts of diethylene glycol butyl ether, 285 parts of white oil, 30 parts of isooctanoic acid, 18 parts of benzoic acid, 50 parts of p-tert-butyl benzoic acid, 20 parts of zinc oxide, 90 parts of barium hydroxide monohydrate, 40 parts of an antioxidant, 162 parts of phosphite ester and 1076 parts of an antioxidant.
A preparation method of a liquid barium-zinc composite stabilizer comprises the following steps:
(1) Preheating: introducing heat conducting oil into a jacket of the reaction kettle, heating the reaction kettle to preheat the reaction kettle to 90 ℃, and starting a stirring mechanism in the reaction kettle;
(2) The raw materials are added for the first time: starting a vacuum pump, and pumping 185 parts of liquid raw materials including oleic acid, diethylene glycol butyl ether, isooctanoic acid and white oil;
(3) Heating, and sequentially adding the following raw materials for the second time and the third time: adding benzoic acid and p-tert-butyl benzoic acid when the temperature is raised to 35 ℃, and adding zinc oxide and barium hydroxide monohydrate when the temperature is raised to 55 ℃;
(4) Secondary heating and heat preservation: when the temperature is raised to 105 ℃, the conduction oil is closed, the temperature is kept for 40 minutes, and the composition in the reaction kettle is changed from white turbidity to clear transparency through an observation sight glass of the reaction kettle;
(5) And (3) heating again and preserving heat: introducing heat conducting oil again to heat the reaction kettle, turning off heating when the temperature is raised to 135 ℃, and continuing to keep the temperature for 35 minutes when the temperature is raised to 140 ℃;
(6) And (3) correction: vacuumizing for 10 minutes, and weighing the discharged water, wherein the weight of the water is 35kg;
(7) And (3) finally adding and stirring the raw materials: adding 100 parts of antioxidant, phosphite ester and white oil, and continuously stirring for 30 minutes;
(8) Returning liquid and barreling: returning the liquid, cooling to 80 ℃, filtering the clear filtrate, and barreling.
Example 3
The liquid barium-zinc composite stabilizer is prepared from the following raw materials, by weight, 190 parts of oleic acid, 90 parts of diethylene glycol butyl ether, 300 parts of white oil, 40 parts of isooctanoic acid, 25 parts of benzoic acid, 35 parts of p-tert-butyl benzoic acid, 17 parts of zinc oxide, 120 parts of barium hydroxide monohydrate, 38 parts of an antioxidant, 180 parts of phosphite ester and 1076 as the antioxidant.
A preparation method of a liquid barium-zinc composite stabilizer comprises the following steps:
(1) Preheating: introducing heat conducting oil into a jacket of the reaction kettle, heating the reaction kettle to preheat the reaction kettle to 110 ℃, and starting a stirring mechanism in the reaction kettle;
(2) The raw materials are added for the first time: turning on a vacuum pump, and pumping 200 parts of liquid raw materials of oleic acid, diethylene glycol butyl ether, isooctanoic acid and white oil;
(3) Heating, and sequentially adding the following raw materials for the second time and the third time: adding benzoic acid and p-tert-butyl benzoic acid when the temperature is raised to 35 ℃, and adding zinc oxide and barium hydroxide monohydrate when the temperature is raised to 60 ℃;
(4) Secondary heating and heat preservation: when the temperature is raised to 100 ℃, the conduction oil is closed, the temperature is kept for 40 minutes, and the composition in the reaction kettle is changed from white turbidity to clear transparency through an observation sight glass of the reaction kettle;
(5) Heating again and preserving heat: introducing heat conducting oil again to heat the reaction kettle, turning off heating when the temperature is raised to 135 ℃, and continuing to preserve heat for 30 minutes when the temperature is raised to 142 ℃;
(6) And (3) correction: vacuumizing for 10 minutes, and weighing the discharged water, wherein the weight of the water is 35kg;
(7) And (3) finally adding and stirring the raw materials: adding 100 parts of antioxidant, phosphite ester and white oil, and continuously stirring for 30 minutes;
(8) Returning liquid and barreling: returning the liquid, cooling to 85 ℃, filtering the clear filtrate, and barreling.
Example 4
The liquid barium-zinc composite stabilizer is prepared from the following raw materials, by weight, 200 parts of oleic acid, 120 parts of diethylene glycol butyl ether, 340 parts of white oil, 25 parts of isooctanoic acid, 30 parts of benzoic acid, 30 parts of p-tert-butyl benzoic acid, 15 parts of zinc oxide, 110 parts of barium hydroxide monohydrate, 25 parts of an antioxidant, 140 parts of phosphite ester and 1076 serving as the antioxidant.
A preparation method of a liquid barium-zinc composite stabilizer comprises the following steps:
(1) Preheating: introducing heat conducting oil into a jacket of the reaction kettle, heating the reaction kettle to preheat the reaction kettle to 120 ℃, and starting a stirring mechanism in the reaction kettle;
(2) The raw materials are added for the first time: opening a vacuum pump, and pumping 240 parts of liquid raw materials of oleic acid, diethylene glycol butyl ether, isooctanoic acid and white oil;
(3) Heating, and sequentially adding the following raw materials for the second time and the third time: adding benzoic acid and p-tert-butyl benzoic acid when the temperature is raised to 45 ℃, and adding zinc oxide and barium hydroxide monohydrate when the temperature is raised to 65 ℃;
(4) Secondary heating and heat preservation: when the temperature is raised to 95 ℃, the conduction oil is closed, the temperature is kept for 35 minutes, and the composition in the reaction kettle is changed from white turbidity to clear transparency through an observation sight glass of the reaction kettle;
(5) Heating again and preserving heat: introducing heat conducting oil again to heat the reaction kettle, turning off heating when the temperature is raised to 130 ℃, and continuing to preserve heat for 40 minutes when the temperature is raised to 135 ℃;
(6) And (3) correction: vacuumizing for 12 minutes, and weighing the discharged water, wherein the weight of the water is 35kg;
(7) And (3) finally adding and stirring the raw materials: adding 100 parts of antioxidant, phosphite ester and white oil, and continuously stirring for 35 minutes;
(8) Returning liquid and barreling: returning the liquid, cooling to 85 ℃, filtering and barreling after the filtrate is clear.
Detection formula
The PVC film is used for preparing a PVC film, the specific formula comprises 65 parts of PVC resin powder, 22 parts of plasticizer, 3 parts of soybean oil, 3 parts of ultramarine and 1.3 parts of liquid barium-zinc composite stabilizer prepared in examples 1-4, and the prepared PVC film is detected in stability, colorability, transparency and precipitation, and the test results are shown in the following table 1:
table 1: test formulations of the stabilizers prepared in examples 1-4 for the same PVC film
From the test results in table 1, it can be seen that: when the liquid barium-zinc composite stabilizer prepared in the embodiments 1 to 4 is used for preparing a PVC film, the liquid barium-zinc composite stabilizer has strong stability, good colorability and high transparency, and can meet the transparency requirement of the PVC film.
According to the liquid barium-zinc composite stabilizer provided by the invention, isooctanoic acid and oleic acid are multi-carbon organic acids, so that the liquid barium-zinc composite stabilizer can play a role in thermal stability and lubricity in preparation, and the thermal stability of a product is improved; diethylene glycol monobutyl ether is used as a diluent to play a role in assisting the complete reaction of metal oxide (zinc oxide), an antioxidant 1076 and phosphite ester are respectively used as the antioxidant and an auxiliary oxidant, p-tert-butyl benzoic acid is used as an organic synthesis intermediate, white oil is beneficial to increasing the brightness of a product, the color of the product is obvious, and benzoic acid is used as a plasticizer. Compared with the similar products on the market, the product has the advantages of strong stability, good colorability, high transparency, competitiveness and strong practicability.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are intended to be within the scope of the invention.
Claims (9)
1. The liquid barium-zinc composite stabilizer is characterized in that raw materials for preparing the liquid barium-zinc composite stabilizer comprise, by weight, 190-240 parts of oleic acid, 90-120 parts of diethylene glycol monobutyl ether, 25-40 parts of isooctanoic acid, 30-50 parts of p-tert-butylbenzoic acid, 15-20 parts of zinc oxide, 90-120 parts of barium hydroxide monohydrate, 25-40 parts of an antioxidant and 140-180 parts of phosphite ester.
2. The liquid barium-zinc composite stabilizer according to claim 1, wherein the oleic acid and the isooctanoic acid are both polycarbonic organic acids, and both of them play roles in thermal stability and lubricity during preparation.
3. The composite stabilizer of claim 1, wherein the diethylene glycol butyl ether is used as a diluent to assist the complete reaction of the metal oxide.
4. The composite stabilizer of claim 1, wherein the antioxidant is 1076, and the phosphite ester is a secondary antioxidant.
5. The liquid barium-zinc composite stabilizer according to claim 1, wherein the raw material components further comprise white oil, and the white oil is 285-340 parts by weight.
6. The liquid barium-zinc composite stabilizer according to claim 5, characterized in that the raw material components further comprise benzoic acid, and the benzoic acid is 18-30 parts by weight.
7. The method for preparing the liquid barium-zinc composite stabilizer according to any one of claims 1 to 6, which is characterized by comprising the following steps:
(1) Preheating: introducing heat-conducting oil into a jacket of the reaction kettle, heating and preheating the reaction kettle, and starting a stirring mechanism in the reaction kettle;
(2) The raw materials are added for the first time: opening a vacuum pump, and pumping liquid raw materials of oleic acid, diethylene glycol butyl ether, isooctanoic acid and white oil;
(3) Heating, and sequentially adding the following raw materials for the second time and the third time: adding benzoic acid and p-tert-butyl benzoic acid when the temperature is raised to 35-45 ℃, and adding zinc oxide and barium hydroxide monohydrate when the temperature is raised to 55-65 ℃;
(4) Secondary heating and heat preservation: when the temperature is increased to 95-105 ℃, the conduction oil is closed, the temperature is kept for 30-40 minutes, and the composition in the reaction kettle is changed from white turbidity to clear transparency through an observation sight glass of the reaction kettle;
(5) Heating again and preserving heat: introducing heat conducting oil again to heat the reaction kettle, closing heating when the temperature is raised to 130-135 ℃, and continuing to preserve heat for 30-40 minutes when the temperature is raised to 135-140 ℃;
(6) And (3) correction: vacuumizing for 10-12 minutes, weighing the discharged water, and supplementing white oil to the part exceeding 35kg;
(7) Finally, feeding and stirring raw materials: adding an antioxidant, phosphite ester, white oil and the white oil supplemented in the step (6), and continuously stirring;
(8) Returning liquid and barreling: returning the liquid, cooling to 80-85 ℃, filtering the filtrate after the filtrate is clear, and barreling.
8. The method for preparing the liquid barium-zinc composite stabilizer according to claim 7, wherein the preheating in the step (1) is to 90-120 ℃.
9. The method for preparing a liquid barium-zinc composite stabilizer according to claim 8, wherein the stirring time in the step (7) is 30 to 35 minutes.
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| CN104910414A (en) * | 2015-06-18 | 2015-09-16 | 巢湖香枫塑胶助剂有限公司 | Preparation method of liquid barium-zinc composite heat stabilizer |
| CN109293988A (en) * | 2018-10-07 | 2019-02-01 | 德清县东来化学有限公司 | A kind of environment-friendly liquid barium zinc compound stabilizer and preparation method thereof |
| CN111499924A (en) * | 2020-05-25 | 2020-08-07 | 德清县东来化学有限公司 | Improved barium-zinc liquid stabilizer and preparation method and application thereof |
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