CN101735481A - Organic calcium-zinc soap lye stabilizing agent - Google Patents
Organic calcium-zinc soap lye stabilizing agent Download PDFInfo
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- CN101735481A CN101735481A CN201010022558A CN201010022558A CN101735481A CN 101735481 A CN101735481 A CN 101735481A CN 201010022558 A CN201010022558 A CN 201010022558A CN 201010022558 A CN201010022558 A CN 201010022558A CN 101735481 A CN101735481 A CN 101735481A
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Abstract
The invention relates to the technical field of PVC thermal stabilizing agents, in particular to an organic calcium-zinc soap lye stabilizing agent. The organic calcium-zinc soap lye stabilizing agent is characterized in that: after calcium superphosphate accounting for 1 to 10 percent of the total weight of raw materials is added into the raw materials, the mixture is thrown into a reactor and stirred for one hour to prepare the organic calcium-zinc soap lye stabilizing agent, wherein the raw materials comprise 34.92 weight percent of zinc stearate, 39.68 weight percent of calcium stearate, 7.94 weight percent of beta-diketone salt, 9.52 weight percent of hydrotalcite and 7.94 weight percent of lube. Compared with the prior art, the calcium superphosphate is added into the raw materials to greatly improve the thermal stability and the lubrication of a PVC product; and the PVC thermal stabilizing agent has the advantages of no toxicity, environmental protection, cheap raw materials, simple preparation method and wide developing space.
Description
[technical field]
The present invention relates to PVC thermo-stabilizer technical field, relate in particular to a kind of organic calcium-zinc soap lye stabilizing agent.
[background technology]
PVC is one of main general-purpose plastics, and many advantages are arranged, but therefore its poor heat stability is added thermo-stabilizer and just become the main method that addresses this problem in PVC processing.
The research and the production of China's thermo-stabilizer start from the 1950's, and stablizers such as initial stage eighties organotin are continually developed and produced, and its industrial structure basically forms.Especially near more than ten years, the consumption of China's thermo-stabilizer also increases considerably along with the fast development of PVC industry.According to incompletely statistics, China's thermo-stabilizer output is about 100,000 t/ at present, 70 families of manufacturer can produce 40～50 kinds of various thermo-stabilizers, and primary categories has lead salts (three salt and two salts etc.), metallic soap of stearic acid class, one package stabilizer, organic tin and organic auxiliary stabilizer etc.Lead salts in the thermo-stabilizer product mainly is that lead sulfate tribasic, second base lead sulfate class account for 39%, and stearates mainly contains salts such as lead stearate, calcium, tin, zinc and accounts for 35%, and organic tin accounts for 5%, and the composite fluid class accounts for 10%, and all the other are 8%.China's thermo-stabilizer product specification is not high at present, and high malicious product is still occupied an leading position, and the middle and high shelves of environment-friendly type thermo-stabilizer product is still produced product based on import or in China's foreign Investment enterprise.
From the nineties in 20th century, in the world, especially western countries forbid that the cry of toxic metal such as leaded in the thermo-stabilizer, cadmium grows to even greater heights.On January 27th, 2003, European Union formally announced " scrap electronic and electrical equipment instruction " (WEEE) and " about in electronic electric equipment, banning use of some objectionable impurities instruction " (RolS).Command request is from July 1st, 2006, forbid European Union's market sale contain lead, mercury, cadmium ,+electronic electric equipment of 6 valency chromium, Polybrominated biphenyl and 6 kinds of objectionable impuritiess of polybromodiphenyl ether; In May, 2006, ESPA and EuPC promise to undertake that jointly European Union will completely forbid the leaded PVC stablizer of use in 2015, and the Vinyl2010 of European Union has also forbidden containing the use of cadmium stabilizer the year ends 2006.Therefore, at present worldwide, nontoxic, pollution-free, compound and efficiently become the irreversible development trend of PVC thermo-stabilizer, and nontoxic Ca/Zn thermo-stabilizer is nontoxic, the environment-friendly type thermo-stabilizer of generally acknowledging in the world, and have advantages such as cheap, that oilness is good, have extremely wide development space.
At present, the main raw material of general Ca/Zn composite thermal stabilizer is: Zinic stearas, calcium stearate, oxidation inhibitor, auxiliary stabilizer, lubricant etc.For Ca-Zn composite heat stabilizer, zinc soap replaces unsettled chlorine atom generation ZnCl on the PVC chain by ester group
2, and ZnCl
2Promote to take off HCl, along with blackening phenomena promptly so-called " zinc burning " rapidly can take place in the prolongation that is subjected to thermal process.
[summary of the invention]
The objective of the invention is to overcome the deficiencies in the prior art, in original raw material, add the thermostability that calcium superphosphate improves the PVC goods.
For achieving the above object, the present invention designs a kind of organic calcium-zinc soap lye stabilizing agent, it is characterized in that: put in the reactor after in batching, adding the calcium superphosphate that accounts for batching gross weight 1%～10%, stir gained after 1 hour, described batching is Zinic stearas 34.92wt%, calcium stearate 39.68wt%, beta diketone 7.94%, hydrotalcite 9.52wt%, lubricant 7.94wt%.
The present invention compares with prior art, has added thermostability, oilness that calcium superphosphate has improved the PVC goods greatly in raw material, nontoxic, environmental protection, and raw material is cheap, and the preparation method is simple, have development space.
[embodiment]
Below in conjunction with embodiment the present invention is further described.
One, batching:
Calcium stearate, Zinic stearas, industrial goods, chemical plant, Nanjing, Nanjing;
Beta diketone;
Hydrotalcite, industrial goods, commercially available;
Lubricant: stearic acid, industrial goods, Hangzhou Oil and Fat Chemical Co., Ltd.;
Two, adopt original prepared thermo-stabilizer 1
#:
With Zinic stearas 22g, calcium stearate 25g, beta diketone 5g, hydrotalcite 6g, lubricant 5g mix in the input reactor, stir 1h, get thermo-stabilizer 1
#
Three, preparation test samples
1, test raw material and major equipment:
SG-3 type polyvinyl chloride resin, Henan Haohua Yuhang Chemical Co., Ltd.;
Softening agent: dioctyl phthalate (DOP) (DOP), industrial goods, peaking worker company limited is closed in the Kunshan;
Weighting agent: treated carbonates, industrial goods, Xuefeng Calcium Carbonate Co., Ltd., Zhejiang;
Double roller plastic-making device, XH-401 type, tin China detecting instrument company limited;
Electronic vulcanizing/forming machine, XH-406, tin China detecting instrument company limited;
Thermostatic oil bath, the GT-7040-M type;
The thermal ageing test case, DHG-9140A type, the grand experimental installation of last Nereid company limited.
Embodiment 1
1, new Recipe prepares thermo-stabilizer 2 in this example
#:
With Zinic stearas 22g, calcium stearate 25g, beta diketone 5g, hydrotalcite 6g, lubricant 5g, calcium superphosphate 0.63g mix in the input reactor, stir 1h, get thermo-stabilizer 2
#
2, specimen preparation
The requirement of corresponding CABLE MATERIALS standard GB/T8815-2202 respectively, J-70 and two cable series of J-50 prescription are tested, the stablizer 1# that has got as having adopted original Recipe preparation among the following table 1-1 makes sample 1 and sample 3 respectively, the stablizer 2# that has got as having adopted new Recipe preparation among the following table 2-1 makes sample 2 and sample 4 respectively.
Table 1-1:
| Batching | ??J-70 | ??J-50 |
| ??PVC | ??100g | ??100g |
| Softening agent (DOP) | ??47g | ??48g |
| Weighting agent | ??45g | ??35g |
| Batching | ??J-70 | ??J-50 |
| Stablizer 1# | ??2g | ??7g |
Table 2-1:
| Batching | ??J-70 | ??J-50 |
| ??PVC | ??100g | ??100g |
| Softening agent (DOP) | ??47g | ??48g |
| Weighting agent | ??45g | ??35g |
| Stablizer 2# | ??2g | ??7g |
Prepare sample respectively by composition of raw materials among above-mentioned table 1-1, the table 2-1, after in polyvinyl chloride resin, adding softening agent, stablizer, after putting into high-speed mixer high-speed stirring to softening agent and blotting fully, add again weighting agent stir the back discharging, be that the discharging of 10～15min rear tab is moulded in refining on 165 ℃ ± 5 ℃ the twin-roll plastic mixing mill with this compound, in temperature is 165 ℃ ± 5 ℃ hydropress, suppress 15～20min depanning in proper order again by the preheating of not pressurizeing, heating and pressurizing, pressurization refrigerative in the roller temperature.
3, sample experiment
(1) Congo red experiment
According to the sample that above-mentioned prescription makes, with reference to the GB/T8815-2202 standard, survey 200 ℃ of Congo red heat-stable times, the results are shown in following table 3-1:
Table 3-1:
By table 3-1 as can be known, the compound heat stabilizer that two classes are different has following result according to 200 ℃ of heat-stable times of standard testing, promptly in J-70 and two serial samples of J-50, stability is respectively by specimen coding: 2＞1,4＞3, and 2 and 4 reach among the GB/T8815-2202 and stipulate, and this result occurring is because after adding calcium superphosphate, the defective of calcium/zinc soap stablizer self is overcome, thereby its stabilization improves.
(2) thermal ageing test
With reference to heat ageing test method in GB GB/T 2915.2-1997 cable insulation and the general test method of sheath material, the sample color of gained is shown in table 4-1:
Table 4-1:
By table 4-1 as can be known, sample 2 and sample 4 have added the thermo-stabilizer of calcium superphosphate, and thermostable effect is better than simple calcium/zinc composite heat stabilizer effect.Especially aspect the long-term thermal stability energy, the compound heat stabilizer that adds people's calcium superphosphate is far better.
Embodiment 2
1, new Recipe prepares thermo-stabilizer 3 in this example
#:
With Zinic stearas 22g, calcium stearate 25g, beta diketone 5g, hydrotalcite 6g, lubricant 5g, calcium superphosphate 1.89g mix in the input reactor, stir 1h, get thermo-stabilizer 3
#
2, specimen preparation
The requirement of corresponding CABLE MATERIALS standard GB/T 8815-2202 respectively, J-70 and two cable series of J-60 prescription are tested, the stablizer 1# that has adopted original prepared among the table 1-2 and got makes sample 5 and sample 7 respectively, the stablizer 2# that has adopted new Recipe preparation among the table 2-2 and got makes sample 6 and sample 8 respectively.
Table 1-2:
| Batching | ??J-70 | ??J-60 |
| ??PVC | ??100g | ??100g |
| Softening agent (DOP) | ??47g | ??48g |
| Weighting agent | ??45g | ??35g |
| Stablizer 1# | ??2g | ??7g |
Table 2-2:
| Batching | ??J-70 | ??J-60 |
| ??PVC | ??100g | ??100g |
| Softening agent (DOP) | ??47g | ??48g |
| Weighting agent | ??45g | ??35g |
| Stablizer 3# | ??2g | ??7g |
Prepare sample respectively by composition of raw materials among above-mentioned table 1-2, the table 2-2, after in polyvinyl chloride resin, adding softening agent, stablizer, after putting into high-speed mixer high-speed stirring to softening agent and blotting fully, add again weighting agent stir the back discharging, be that the discharging of 10～15min rear tab is moulded in refining on 165 ℃ ± 5 ℃ the twin-roll plastic mixing mill with this compound, in temperature is 165 ℃ ± 5 ℃ hydropress, suppress 15～20min depanning in proper order again by the preheating of not pressurizeing, heating and pressurizing, pressurization refrigerative in the roller temperature.
3, sample experiment
(1) Congo red experiment
According to the sample that above-mentioned prescription makes, with reference to the GB/T8815-2202 standard, survey 200 ℃ of Congo red heat-stable times, the results are shown in following table 3-2:
Table 3-2:
By table 3-2 as can be known, the compound heat stabilizer that two classes are different has following result according to 200 ℃ of heat-stable times of standard testing, promptly in J-70 and two serial samples of J-60, stability is respectively by specimen coding: 6＞5,8＞7, and 6 and 8 reach among the GB/T8815-2202 and stipulate, and this result occurring is because after adding calcium superphosphate, the defective of calcium/zinc soap stablizer self is overcome, thereby its stabilization improves.
(2) thermal ageing test
With reference to heat ageing test method in GB GB/T 2915.2-1997 cable insulation and the general test method of sheath material, the sample color of gained is shown in table 4-2:
Table 4-2:
| ??60 | - | Golden yellow | - | Orange |
| ??75 | - | Brown | - | Golden yellow |
| ??90 | - | Dark brown | - | Golden yellow |
| ??105 | - | ??- | - | Brown |
| ??120 | - | ??- | - | Dark brown |
By table 4-2 as can be known, sample 6 and 8 has added the thermo-stabilizer of calcium superphosphate, and thermostable effect is better than simple calcium/zinc composite heat stabilizer effect.Especially aspect the long-term thermal stability energy, the compound heat stabilizer that adds people's calcium superphosphate is far better.
Embodiment 3
1, new Recipe prepares thermo-stabilizer 4 in this example
#
With Zinic stearas 22g, calcium stearate 25g, beta diketone 5g, hydrotalcite 6g, lubricant 5g, calcium superphosphate 3.15g mix in the input reactor, stir 1h, get thermo-stabilizer 4
#
1, specimen preparation
The requirement of corresponding CABLE MATERIALS standard GB/T 8815-2202 respectively, J-70 and two cable series of J-80 prescription are tested, the stablizer 1# that has adopted original prepared among the table 1-3 and got makes sample 9 and sample 11 respectively, the stablizer 2# that has adopted new formulation among the table 2-3 and got makes sample 10 and sample 12 respectively.
Table 1-3:
| Batching | ??J-70 | ??J-80 |
| ??PVC | ??100g | ??100g |
| Softening agent (DOP) | ??47g | ??48g |
| Weighting agent | ??45g | ??35g |
| Batching | ??J-70 | ??J-80 |
| Stablizer 1# | ??2g | ??7g |
Table 2:
| Batching | ??J-70 | ??J-80 |
| ??PVC | ??100g | ??100g |
| Softening agent (DOP) | ??47g | ??48g |
| Weighting agent | ??45g | ??35g |
| Stablizer 4# | ??2g | ??7g |
Prepare sample respectively by composition of raw materials among above-mentioned table 1-3, the table 2-3, after in polyvinyl chloride resin, adding softening agent, stablizer, after putting into high-speed mixer high-speed stirring to softening agent and blotting fully, add again weighting agent stir the back discharging, be that the discharging of 10～15min rear tab is moulded in refining on 165 ℃ ± 5 ℃ the twin-roll plastic mixing mill with this compound, in temperature is 165 ℃ ± 5 ℃ hydropress, suppress 15～20min depanning in proper order again by the preheating of not pressurizeing, heating and pressurizing, pressurization refrigerative in the roller temperature.
3, sample experiment
(1) Congo red experiment
According to the sample that above-mentioned prescription makes, with reference to the GB/T8815-2202 standard, survey 200 ℃ of Congo red heat-stable times, the results are shown in following table 3-3:
Table 3-3:
As shown in Table 3, the compound heat stabilizer that two classes are different has following result according to 200 ℃ of heat-stable times of standard testing, promptly in J-70 and two serial samples of J-80, stability is respectively by specimen coding: 10＞9,12＞11, and 10 and 12 reach among the GB/T8815-2202 and stipulate, and this result occurring is because after adding calcium superphosphate, the defective of calcium/zinc soap stablizer self is overcome, thereby its stabilization improves.
(2) thermal ageing test
With reference to heat ageing test method in GB GB/T 2915.2-1997 cable insulation and the general test method of sheath material, the sample color of gained is shown in table 4-3:
Table 4-3:
By table 4-3 as can be known, sample 10 and 12 has added the thermo-stabilizer of calcium superphosphate, and thermostable effect is better than simple calcium/zinc composite heat stabilizer effect.Especially aspect the long-term thermal stability energy, the compound heat stabilizer that adds people's calcium superphosphate is far better.
Embodiment 4
1, new Recipe prepares thermo-stabilizer 5 in this example
#:
With Zinic stearas 22g, calcium stearate 25g, beta diketone 5g, hydrotalcite 6g, lubricant 5g, calcium superphosphate 6.3g mix in the input reactor, stir 1h, get thermo-stabilizer 5
#
2, specimen preparation
The requirement of corresponding CABLE MATERIALS standard GB/T 8815-2202 respectively, J-70 and two cable series of J-90 prescription are tested, table adopted above-mentioned prepared among the 1-4 and stablizer 1# make sample 13 and sample 15 respectively, adopted above-mentioned prepared among the table 2-4 and stablizer 2# make sample 14 and sample 16 respectively.
Table 1:
| Batching | ??J-70 | ??J-90 |
| ??PVC | ??100g | ??100g |
| Softening agent (DOP) | ??47g | ??48g |
| Weighting agent | ??45g | ??35g |
| Batching | ??J-70 | ??J-90 |
| Stablizer 1# | ??2g | ??7g |
Table 2:
| Batching | ??J-70 | ??J-90 |
| ??PVC | ??100g | ??100g |
| Softening agent (DOP) | ??47g | ??48g |
| Weighting agent | ??45g | ??35g |
| Stablizer 5# | ??2g | ??7g |
Prepare sample respectively by the prescription among above-mentioned table 1-4, the table 2-4, after in polyvinyl chloride resin, adding softening agent, stablizer, after putting into high-speed mixer high-speed stirring to softening agent and blotting fully, add again weighting agent stir the back discharging, be that the discharging of 10～15min rear tab is moulded in refining on 165 ℃ ± 5 ℃ the twin-roll plastic mixing mill with this compound, in temperature is 165 ℃ ± 5 ℃ hydropress, suppress 15～20min depanning in proper order again by the preheating of not pressurizeing, heating and pressurizing, pressurization refrigerative in the roller temperature.
3, sample experiment
(1) Congo red experiment
According to the sample that above-mentioned prescription makes, with reference to the GB/T8815-2202 standard, survey 200 ℃ of Congo red heat-stable times, the results are shown in following table 3-4:
Table 3:
| Sample | The CABLE MATERIALS model | Stablizer | 200 ℃ of thermostability time/min | Technical indicator/min |
| ??13 | ??J-70 | ??1 # | ??50 | ??≥60 |
By table 3-4 as can be known, the compound heat stabilizer that two classes are different has following result according to 200 ℃ of heat-stable times of standard testing, promptly in J-70 and two serial samples of J-90, stability is respectively by specimen coding: 14＞13,16＞15, and 14 and 16 reach among the GB/T8815-2202 and stipulate, and this result occurring is because after adding calcium superphosphate, the defective of calcium/zinc soap stablizer self is overcome, thereby its stabilization improves.
(2) thermal ageing test
With reference to heat ageing test method in GB GB/T 2915.2-1997 cable insulation and the general test method of sheath material, the sample color of gained is shown in table 4-4:
Table 4-4:
By table 4-4 as can be known, sample 14 and 16 has added the thermo-stabilizer of calcium superphosphate, and thermostable effect is better than simple calcium/zinc composite heat stabilizer effect.Especially aspect the long-term thermal stability energy, the compound heat stabilizer that adds people's calcium superphosphate is far better.
By experiment showed, in the foregoing description that calcium/zinc soap composite thermal stabilizer of containing calcium superphosphate heat stabilization to the PVC CABLE MATERIALS is better than traditional calcium/zinc soap one package stabilizer.
Claims (1)
1. organic calcium-zinc soap lye stabilizing agent, it is characterized in that: put in the reactor after in batching, adding the calcium superphosphate that accounts for batching gross weight 1%～10%, stir obtained after 1 hour, described batching is Zinic stearas 34.92wt%, calcium stearate 39.68wt%, beta diketone 7.94wt%, hydrotalcite 9.52wt%, lubricant 7.94wt%.
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101967253A (en) * | 2010-10-26 | 2011-02-09 | 湘乡市贝特尔塑胶有限公司 | Environmentally-friendly PVC calcium zinc composite stabilizer |
| CN102477196A (en) * | 2010-11-30 | 2012-05-30 | 山东慧科助剂股份有限公司 | Novel molecular sieve PVC composite stabilizing agent and its preparation method |
| CN102977410A (en) * | 2012-12-15 | 2013-03-20 | 新郑市庆宏化工有限公司 | Calcium-zinc composite heat stabilizer and preparation method thereof |
| CN103694599A (en) * | 2013-12-11 | 2014-04-02 | 甘肃大禹节水集团股份有限公司 | Efficient and environment-friendly polyvinyl chloride heat stabilizer and preparation method thereof |
-
2010
- 2010-01-06 CN CN201010022558A patent/CN101735481A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101967253A (en) * | 2010-10-26 | 2011-02-09 | 湘乡市贝特尔塑胶有限公司 | Environmentally-friendly PVC calcium zinc composite stabilizer |
| CN102477196A (en) * | 2010-11-30 | 2012-05-30 | 山东慧科助剂股份有限公司 | Novel molecular sieve PVC composite stabilizing agent and its preparation method |
| CN102477196B (en) * | 2010-11-30 | 2014-01-29 | 山东慧科助剂股份有限公司 | Novel molecular sieve PVC composite stabilizing agent and its preparation method |
| CN102977410A (en) * | 2012-12-15 | 2013-03-20 | 新郑市庆宏化工有限公司 | Calcium-zinc composite heat stabilizer and preparation method thereof |
| CN103694599A (en) * | 2013-12-11 | 2014-04-02 | 甘肃大禹节水集团股份有限公司 | Efficient and environment-friendly polyvinyl chloride heat stabilizer and preparation method thereof |
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Application publication date: 20100616 |