CN108948427A - A kind of PVC heat-resistant stable agent and preparation method thereof - Google Patents
A kind of PVC heat-resistant stable agent and preparation method thereof Download PDFInfo
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- CN108948427A CN108948427A CN201810898271.1A CN201810898271A CN108948427A CN 108948427 A CN108948427 A CN 108948427A CN 201810898271 A CN201810898271 A CN 201810898271A CN 108948427 A CN108948427 A CN 108948427A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The present invention relates to plastic additive technical fields, specifically disclose a kind of PVC heat-resistant stable agent and preparation method thereof.The stabilizer, the raw material components comprising following parts by weight: 50~100 parts of alumina silicate；20~50 parts of titanium dioxide；20~50 parts of calcium stearate.The stabilizer is a kind of stabilizer completely newly formed, and embodiment test proves that the stabilizer has good high-temperature resistant result.
Description
Technical field
The present invention relates to plastic additive technical fields, and in particular to a kind of PVC heat-resistant stable agent and its preparation side
Method.
Background technique
Polyvinyl chloride (PVC) is the white powder of amorphous structure, is a kind of using in a chlorine atom substitution polyethylene
A hydrogen atom high molecular material, be the amorphous polymer containing a small amount of crystalline texture.It is in construction material, industry system
Product, floor tile, tubing etc. are widely used.
But 77~90 DEG C of the glass transition temperature of PVC, 170 DEG C or so start to decompose, to heat stability it is poor, 100 DEG C with
On, it will decompose and generate hydrogen chloride, and further autocatalysis is decomposed, and causes to change colour, physical mechanical property also declines rapidly,
Therefore, it must be added to stabilizer in practical applications to improve the stability to heat.
But the type of the current heat stabilizer for PVC is not very much.Therefore, further exploitation is steady for the heat of PVC
Agent is determined with important market prospects.
Summary of the invention
The technical problem to be solved by the invention is to provide a kind of PVC heat-resistant stable agent and preparation method thereof.This hair
The bright PVC has excellent high temperature resistance with heat-resistant stable agent.
Above-mentioned technical problem to be solved by this invention, is achieved by the following technical programs:
A kind of PVC heat-resistant stable agent, it includes the raw material components of following parts by weight:
50~100 parts of alumina silicate；20~50 parts of titanium dioxide；20~50 parts of calcium stearate.
Preferably, PVC heat-resistant stable agent, it includes the raw material components of following parts by weight:
70~90 parts of alumina silicate；30~40 parts of titanium dioxide；30~40 parts of calcium stearate.
Preferably, PVC heat-resistant stable agent, it includes the raw material components of following parts by weight for a most step:
80 parts of alumina silicate；30 parts of titanium dioxide；30 parts of calcium stearate.
As it is known by the man skilled in the art that the selection of the high-temperature resistant result and raw material of stabilizer and proportion are closely related；
The selection and proportion collocation of raw material are bad, although can be prepared has certain stabilizer resistant to high temperature, effect cannot be fine,
The superposition of only several raw material high-temperature resistant results.And if the selection of raw material and ratio collocation optimize, stabilizer
The high-temperature resistant result for playing each ingredient can be cooperateed with.Inventor is largely had found through a large amount of experimental study, by silicon
The stabilizer that sour aluminium, titanium dioxide and calcium stearate three are prepared after mixing according to the above ratio is imitated with preferable high temperature resistant
Fruit.
The present invention also provides a kind of above-mentioned PVC preparation methods of heat-resistant stable agent, and it includes following steps:
(1) 3~6h of immersion in mixed acid solution is put into after mixing raw material alumina silicate, titanium dioxide and calcium stearate, clearly
Sour processed raw material is obtained in water after washing to neutrality；
(2) the processed raw material of acid is added to the water, adjusting PH is 8~9, and Ammonium Acetate is then added；At 50~60 DEG C
React 8~12h；
(3) it is separated by solid-liquid separation after reaction, washs solid, then is steady up to the PVC high temperature resistant after drying
Determine agent.
Preferably, mixed acid solution described in step (1) is the mixed acid solution that the concentrated sulfuric acid and concentrated nitric acid form.
Most preferably, the volumetric usage of the concentrated sulfuric acid and concentrated nitric acid ratio is 3:1.
Preferably, the weight consumption of water is 3~5 times of the processed raw material gross weight of acid in step (2).
Most preferably, the weight consumption of water is 4 times of the processed raw material gross weight of acid in step (2).
Preferably, the weight consumption of Ammonium Acetate is the 1/10~1/5 of the processed raw material gross weight of acid in step (2).
Most preferably, the weight consumption of Ammonium Acetate is the 1/8 of the processed raw material gross weight of acid in step (2).
Researcher of the present invention also found that the preparation method of stabilizer is also further influence stabilizer high-temperature resistant result
One key factor.The present invention further study show that, the stabilizer being prepared under above-mentioned preparation method, high temperature resistant effect
Fruit is further promoted.
The utility model has the advantages that embodiment test proves the stabilizer the present invention provides the stabilizer that one kind completely newly forms
With good high-temperature resistant result；The stabilizer being especially prepared under the method for the invention, high-temperature resistant result is more
Significantly.
Specific embodiment
The present invention is explained further below in conjunction with specific embodiment, but embodiment does not do any type of limit to the present invention
It is fixed.
The preparation of embodiment 1PVC heat-resistant stable agent
Parts by weight composition: 80 parts of alumina silicate；30 parts of titanium dioxide；30 parts of calcium stearate.
Preparation method: alumina silicate, titanium dioxide and calcium stearate are uniformly mixed to obtain the final product.
The preparation of embodiment 2PVC heat-resistant stable agent
Parts by weight composition: 70 parts of alumina silicate；40 parts of titanium dioxide；30 parts of calcium stearate.
Preparation method: alumina silicate, titanium dioxide and calcium stearate are uniformly mixed to obtain the final product.
The preparation of embodiment 3PVC heat-resistant stable agent
Parts by weight composition: 90 parts of alumina silicate；30 parts of titanium dioxide；40 parts of calcium stearate.
Preparation method: alumina silicate, titanium dioxide and calcium stearate are uniformly mixed to obtain the final product.
The preparation of embodiment 4PVC heat-resistant stable agent
Parts by weight composition: 80 parts of alumina silicate；30 parts of titanium dioxide；30 parts of calcium stearate.
Preparation method: (1) it is put into mixed acid solution and impregnates after mixing raw material alumina silicate, titanium dioxide and calcium stearate
5h, in clear water after washing to neutrality sour processed raw material；
(2) the processed raw material of acid is added to the water, adjusting PH is 8.5, and Ammonium Acetate is then added；It is reacted at 55 DEG C
10h；
(3) it is separated by solid-liquid separation after reaction, washs solid, then is steady up to the PVC high temperature resistant after drying
Determine agent；
Mixed acid solution described in step (1) is the mixed acid solution that the concentrated sulfuric acid and concentrated nitric acid form；The concentrated sulfuric acid
Volumetric usage ratio with concentrated nitric acid is 3:1；
The weight consumption of water is 4 times of the processed raw material gross weight of acid in step (2)；
The weight consumption of Ammonium Acetate is the 1/8 of the processed raw material gross weight of acid in step (2).
The preparation of embodiment 5PVC heat-resistant stable agent
Parts by weight composition: 70 parts of alumina silicate；40 parts of titanium dioxide；30 parts of calcium stearate.
Preparation method: (1) it is put into mixed acid solution and impregnates after mixing raw material alumina silicate, titanium dioxide and calcium stearate
3h, in clear water after washing to neutrality sour processed raw material；
(2) the processed raw material of acid is added to the water, adjusting PH is 8, and Ammonium Acetate is then added；12h is reacted at 50 DEG C；
(3) it is separated by solid-liquid separation after reaction, washs solid, then is steady up to the PVC high temperature resistant after drying
Determine agent；
Mixed acid solution described in step (1) is the mixed acid solution that the concentrated sulfuric acid and concentrated nitric acid form；The concentrated sulfuric acid
Volumetric usage ratio with concentrated nitric acid is 3:1；
The weight consumption of water is 3 times of the processed raw material gross weight of acid in step (2)；
The weight consumption of Ammonium Acetate is the 1/5 of the processed raw material gross weight of acid in step (2).
The preparation of embodiment 6PVC heat-resistant stable agent
Parts by weight composition: 90 parts of alumina silicate；30 parts of titanium dioxide；40 parts of calcium stearate.
Preparation method: (1) it is put into mixed acid solution and impregnates after mixing raw material alumina silicate, titanium dioxide and calcium stearate
6h, in clear water after washing to neutrality sour processed raw material；
(2) the processed raw material of acid is added to the water, adjusting PH is 9, and Ammonium Acetate is then added；8h is reacted at 60 DEG C；
(3) it is separated by solid-liquid separation after reaction, washs solid, then is steady up to the PVC high temperature resistant after drying
Determine agent；
Mixed acid solution described in step (1) is the mixed acid solution that the concentrated sulfuric acid and concentrated nitric acid form；The concentrated sulfuric acid
Volumetric usage ratio with concentrated nitric acid is 3:1；
The weight consumption of water is 5 times of the processed raw material gross weight of acid in step (2)；
The weight consumption of Ammonium Acetate is the 1/10 of the processed raw material gross weight of acid in step (2).
The preparation of 1 stabilizer of comparative example
Parts by weight composition: 80 parts of alumina silicate；30 parts of titanium dioxide.
Preparation method: alumina silicate, titanium dioxide are uniformly mixed to obtain the final product.
The preparation of 2 stabilizer of comparative example
Parts by weight composition: 30 parts of titanium dioxide；30 parts of calcium stearate.
Preparation method: titanium dioxide, calcium stearate are uniformly mixed to obtain the final product.
The preparation of 3 stabilizer of comparative example
Parts by weight composition: 80 parts of alumina silicate；30 parts of calcium stearate.
Preparation method: alumina silicate, calcium stearate are uniformly mixed to obtain the final product.
The preparation of 4 stabilizer of comparative example
Parts by weight composition: 80 parts of alumina silicate；30 parts of titanium dioxide.
Preparation method: (1) it is put into mixed acid solution after mixing raw material alumina silicate, titanium dioxide and impregnates 6h, in clear water
Sour processed raw material is obtained after washing to neutrality；
(2) the processed raw material of acid is added to the water, adjusting PH is 9, and Ammonium Acetate is then added；8h is reacted at 60 DEG C；
(3) it is separated by solid-liquid separation after reaction, washs solid, then is steady up to the PVC high temperature resistant after drying
Determine agent；
Mixed acid solution described in step (1) is the mixed acid solution that the concentrated sulfuric acid and concentrated nitric acid form；The concentrated sulfuric acid
Volumetric usage ratio with concentrated nitric acid is 3:1；
The weight consumption of water is 5 times of the processed raw material gross weight of acid in step (2)；
The weight consumption of Ammonium Acetate is the 1/10 of the processed raw material gross weight of acid in step (2).
7 heat stability testing of embodiment
By the stabilizer that Examples 1 to 6 is prepared and the stabilizer that comparative example 1~4 is prepared, with PVC by weight
Amount than be 0.5:99.5 than mixed at high speed 3min after, referring to conventional method, sufficiently plasticate, make on plasticator in 180~190 DEG C
It is standby to obtain PVC material 1~10.PVC material 1~10 is subjected to static and dynamic thermal stability time test.The specific method is as follows: pressing
According to PVC heat stability testing method-congo red method as defined in GB3917-1982, in 190 DEG C of progress static heat stability tests.
Dynamic thermal stability test is carried out under the conditions of 190 DEG C according to torque rheometer experiment.Test result is shown in Table 1:
1. heat stability testing of table
Examples 1 to 3 is compared with comparative example 1~3 it can be seen from 1 test data of table, what Examples 1 to 3 was prepared
The static heat-stable time and dynamic heat-stable time of stabilizer are that the static heat for the stabilizer that comparative example 1~3 is prepared is steady
2 times to fix time with dynamic heat-stable time.This explanation is by raw material alumina silicate, titanium dioxide and calcium stearate by of the present invention
The mixed heat-resisting effect of ratio both will be any far better than raw material alumina silicate, titanium dioxide and calcium stearate mixing；
The mixing of raw material alumina silicate, titanium dioxide and calcium stearate three can cooperate with performance heat-resisting effect.
In addition, embodiment 4~6, compared with Examples 1 to 3, the static heat for the stabilizer that embodiment 4~6 is prepared is steady
Fixing time is the static heat-stable time and Dynamic Thermal for the stabilizer that Examples 1 to 3 is prepared again with dynamic heat-stable time
Stablize 2 times of time.Raw material alumina silicate, titanium dioxide and calcium stearate are prepared this explanation in accordance with the method for the present invention
Stabilizer its heat-resisting effect than raw material alumina silicate, titanium dioxide and calcium stearate to be simply mixed to the stabilizer being prepared
It is more significant.In addition, can be seen that from 4 test data of comparative example two kinds of alumina silicate, titanium dioxide raw materials are mixed after by the present invention
The stabilizer that the method is prepared, heat-resisting effect can not be substantially improved as embodiment 4~6.
Claims (10)
1. a kind of PVC heat-resistant stable agent, which is characterized in that the raw material components comprising following parts by weight:
50~100 parts of alumina silicate；20~50 parts of titanium dioxide；20~50 parts of calcium stearate.
2. PVC according to claim 1 heat-resistant stable agent, which is characterized in that the raw material group comprising following parts by weight
Point:
70~90 parts of alumina silicate；30~40 parts of titanium dioxide；30~40 parts of calcium stearate.
3. PVC according to claim 2 heat-resistant stable agent, which is characterized in that the raw material group comprising following parts by weight
Point:
80 parts of alumina silicate；30 parts of titanium dioxide；30 parts of calcium stearate.
4. the preparation method of claims 1 to 3 described in any item PVC heat-resistant stable agent, which is characterized in that comprising as follows
Step:
(1) it is put into after mixing raw material alumina silicate, titanium dioxide and calcium stearate in mixed acid solution and impregnates 3~6h, in clear water
Sour processed raw material is obtained after washing to neutrality；
(2) the processed raw material of acid is added to the water, adjusting PH is 8~9, and Ammonium Acetate is then added；8 are reacted at 50~60 DEG C
~12h；
(3) it is separated by solid-liquid separation after reaction, washs solid, then after drying up to PVC heat-resistant stable agent.
5. the PVC according to claim 4 preparation method of heat-resistant stable agent, which is characterized in that described in step (1)
Mixed acid solution be mixed acid solution that the concentrated sulfuric acid and concentrated nitric acid form.
6. the PVC according to claim 5 preparation method of heat-resistant stable agent, which is characterized in that the concentrated sulfuric acid and dense nitre
The volumetric usage ratio of acid is 3:1.
7. the PVC according to claim 4 preparation method of heat-resistant stable agent, which is characterized in that water in step (2)
Weight consumption is 3~5 times of the processed raw material gross weight of acid.
8. the PVC according to claim 7 preparation method of heat-resistant stable agent, which is characterized in that water in step (2)
Weight consumption is 4 times of the processed raw material gross weight of acid.
9. the PVC according to claim 4 preparation method of heat-resistant stable agent, which is characterized in that acetyl in step (2)
The weight consumption of ammonium is the 1/10~1/5 of the processed raw material gross weight of acid.
10. the PVC according to claim 9 preparation method of heat-resistant stable agent, which is characterized in that second in step (2)
The weight consumption of acyl ammonium is the 1/8 of the processed raw material gross weight of acid.
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2018
- 2018-08-08 CN CN201810898271.1A patent/CN108948427A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104479260A (en) * | 2015-01-21 | 2015-04-01 | 芜湖海螺型材科技股份有限公司 | PVC sectional material adopting organic tin stabilizer and preparation method of PVC sectional material |
| CN104962098A (en) * | 2015-07-28 | 2015-10-07 | 任新年 | Wear-resistant degradable plastic and preparation method thereof |
| CN107353536A (en) * | 2017-07-18 | 2017-11-17 | 合肥万之景门窗有限公司 | A kind of high durable polychloroethylene section bar for door and window and preparation method thereof |
| CN107857956A (en) * | 2017-12-01 | 2018-03-30 | 合肥华福土工合成材料有限公司 | A kind of plastic-steel window material and preparation method thereof |
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Application publication date: 20181207 |