CN111471328A - Modification method of hydrotalcite powder and application of hydrotalcite powder in calcium-zinc stabilizer - Google Patents
Modification method of hydrotalcite powder and application of hydrotalcite powder in calcium-zinc stabilizer Download PDFInfo
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Abstract
The invention relates to a modification method of hydrotalcite powder and an application step S1 of the hydrotalcite powder in a calcium zinc stabilizer, wherein the method comprises the steps of roughly selecting the raw material hydrotalcite, crushing the hydrotalcite powder to a certain particle size, adding a certain amount of water and a pulping aid to prepare slurry, and the pulping aid is composed of ethylhexyl phosphoric acid, sodium dodecyl sulfate and polyethylene glycol with the molecular weight of 200-600; step S2: purifying; step S3: organic activation, adding a certain amount of organic ammonium salt and an activation aid, and carrying out activation reaction for a certain time, wherein the activation aid is 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride; step S4: filtering, drying, crushing and sieving to obtain the modified hydrotalcite powder. The inventor of the application finds that the modified hydrotalcite powder has a good lubricating component stability effect, and the lubricating components are adsorbed and/or anchored in the modified hydrotalcite powder in a highly dispersed manner, so that precipitation is greatly reduced, and unsmooth PVC-U plates are avoided.
Description
Technical Field
The invention relates to a modification method of hydrotalcite powder and application thereof in a calcium-zinc stabilizer, belonging to the technical field of processing of composite calcium-zinc stabilizers.
Background
PVC is one of five general-purpose plastics, and is widely applied to the fields of industry, building, agriculture and the like. The thermal stability of the product is extremely poor, the color of the product is darkened due to thermal decomposition of the product, various indexes are reduced, and the thermal stability of the product needs to be improved by using a thermal stabilizer.
The calcium-zinc composite stabilizer is a composite stabilizer generated by taking metal soaps and salts such as calcium, zinc and the like as main bodies and adding other auxiliary agents such as phosphite ester and the like, is an environment-friendly stabilizer, is mainly used for PVC-U environment-friendly sectional materials, takes calcium stearate and zinc stearate as main bodies, and has the following defects in the generation of PVC-U sectional materials: 1. needle-shaped precipitation exists in the production process, the glossiness of the product is reduced, and the production stability is poor; 2. the inner cavity of the product is not welded well, the problem of broken ribs is easy to occur, the mould is required to be cleaned at an irregular period, the production efficiency is influenced, and the raw materials are wasted. Hydrotalcite materials belong to anionic layered compounds. The layered compound is a compound with a layered structure, interlayer ions and exchangeability, and some functional object substances are introduced into interlayer gaps and spread the interlayer distance to form a pillared interlayer compound by utilizing the intercalation property of a layered compound host under the action of strong polar molecules and the exchangeability of the interlayer ions. The conventional hydrotalcite powder is used for the calcium-zinc stabilizer, and the problem that lubricating components cannot be separated out is still solved.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provide a method for modifying hydrotalcite powder.
The second purpose of the invention is to solve the defects of the prior art and provide the application of the modified hydrotalcite powder in the calcium zinc stabilizer.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the preparation method of the modified hydrotalcite powder comprises the following steps:
step S1, coarsely selecting raw material hydrotalcite, crushing the hydrotalcite to a certain particle size, adding a certain amount of water and a pulping aid to prepare slurry, wherein the pulping aid is composed of ethylhexyl phosphoric acid, sodium dodecyl sulfate and polyethylene glycol with molecular weight of 200-600-;
step S2: purifying;
step S3: organic activation, adding a certain amount of organic ammonium salt and an activation aid, and carrying out activation reaction for a certain time, wherein the activation aid is 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride;
step S4: filtering, drying, crushing and sieving to obtain the modified hydrotalcite powder.
The calcium-zinc stabilizer has a certain lubricating component, the temperature of the profile is higher when the profile is discharged from a die in the profile extrusion process, the temperature of the sizing die is about 20 ℃ when the profile enters the sizing die at about 200 ℃, the temperature difference between the sizing die and the sizing die is larger, the lubricating component is separated out, the precipitate influences the surface flatness of a product, and the adverse effect is caused on the forming of the product.
The inventor of the application finds that the modified hydrotalcite powder has good lubricating component stability, and specifically comprises the following components: the modified hydrotalcite powder has multiple active sites and can be adsorbed and/or anchored and lubricatedThe method only loses interlayer moisture when the inherent thermal stability of the hydrotalcite powder is lower than 200 ℃ in the air, has no influence on the structure, loses more moisture when heated to 250-450 ℃, and simultaneously has CO2And the generated lubricating components are adsorbed and/or anchored in the modified hydrotalcite powder in a highly dispersed manner, so that the precipitation is greatly reduced, and the unsmooth property of the PVC-U plate is avoided.
Specifically, by modifying hydrotalcite powder, the dispersibility of the slurry can be remarkably improved by the sodium dodecyl sulfate, the wettability of the hydrotalcite raw material can be improved by the combination of the ethylhexyl phosphoric acid and the polyethylene glycol, the hydrotalcite raw material and the pulping water are well mixed, the hydrotalcite raw material and the pulping water are matched and used in a specific dosage, the dispersion performance of the hydrotalcite raw material is improved under the synergistic effect, the viscosity of the slurry is indirectly improved, the viscosity is uniform, and the subsequent organic efficiency and effect are improved.
In the invention, a certain amount of activating auxiliary agents are also added, and the activating auxiliary agents can promote the organic activation reaction, accelerate the organic activation efficiency, improve the organic activation effect and improve the adsorption effect and/or the anchoring effect of the hydrotalcite powder on the lubricating components.
Preferably, the addition amount of the pulping aid is 3-8% of the mass of the raw material hydrotalcite, and the mass ratio of the sodium lignosulfonate in the pulping aid is 30-50%.
Preferably, the addition amount of the pulping aid is 5% of the mass of the raw material hydrotalcite, the mass ratio of the lauryl sodium sulfate in the pulping aid is 30-40%, the mass percentage of the ethylhexyl phosphoric acid is 3-5%, and the balance is polyethylene glycol.
Preferably, the mass ratio of the lauryl sodium sulfate in the pulping assistant is 35%, the mass ratio of the ethylhexyl phosphoric acid is 4%, and the balance is polyethylene glycol.
Preferably, in the organic activation, the organic ammonium salt is one or a mixture of more of dioctadecyl dimethyl ammonium chloride, dioctadecyl dihydroxy ammonium chloride, octadecyl ammonium salt and dodecyl tertiary methyl hydrochloride.
Preferably, the addition amount of the activating assistant is 1-3% of the mass of the raw material hydrotalcite.
Preferably, the addition amount of the activating assistant is 2% by mass of the raw material hydrotalcite.
Preferably, the purification operation is as follows: adding 20-30% ethanol aqueous solution with volume 3-5 times of the slurry in the step S1, stirring uniformly, standing for layering, removing supernatant, and repeating for 1-3 times.
The modified hydrotalcite powder prepared by the preparation method of the modified hydrotalcite powder is applied to a calcium-zinc stabilizer, and the calcium-zinc stabilizer is any one of a PVC-U plate calcium-zinc stabilizer, a PVC pipeline calcium-zinc stabilizer and a PVC wire and cable calcium-zinc stabilizer.
The invention has the beneficial effects that: the inventor of the application finds that the modified hydrotalcite powder has good lubricating component stability, and specifically comprises the following components: the modified hydrotalcite powder has multiple active sites, can adsorb and/or anchor lubricating ingredients, simultaneously uses the inherent thermal stability of hydrotalcite powder, only loses interlayer moisture when the temperature in the air is lower than 200 ℃, has no influence on the structure, loses more moisture when heated to 250-450 ℃, and simultaneously has CO2And the generated lubricating components are adsorbed and/or anchored in the modified hydrotalcite powder in a highly dispersed manner, so that the precipitation is greatly reduced, and the unsmooth property of the PVC-U plate is avoided.
Specifically, by modifying hydrotalcite powder, the dispersibility of the slurry can be remarkably improved by the sodium dodecyl sulfate, the wettability of the hydrotalcite raw material can be improved by the combination of the ethylhexyl phosphoric acid and the polyethylene glycol, the hydrotalcite raw material and the pulping water are well mixed, the hydrotalcite raw material and the pulping water are matched and used in a specific dosage, the dispersion performance of the hydrotalcite raw material is improved under the synergistic effect, the viscosity of the slurry is indirectly improved, the viscosity is uniform, and the subsequent organic efficiency and effect are improved.
In the invention, a certain amount of activating auxiliary agents are also added, and the activating auxiliary agents can promote the organic activation reaction, accelerate the organic activation efficiency, improve the organic activation effect and improve the adsorption effect and/or the anchoring effect of the hydrotalcite powder on the lubricating components.
Detailed Description
The technical solution of the present invention will be further specifically described below by way of specific examples.
Example 1:
the preparation method of the modified hydrotalcite powder comprises the following steps:
step S1, coarsely selecting raw material hydrotalcite, crushing the hydrotalcite to a certain particle size, adding a certain amount of water and a pulping aid to prepare slurry, wherein the pulping aid is composed of ethylhexyl phosphoric acid, sodium dodecyl sulfate and polyethylene glycol with molecular weight of 200;
step S2: purifying;
step S3: organic activation, adding a certain amount of organic ammonium salt and an activation aid, and carrying out activation reaction for a certain time, wherein the activation aid is 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride;
step S4: filtering, drying, crushing and sieving to obtain the modified hydrotalcite powder.
In the invention, the addition amount of the pulping aid is 3% of the mass of the raw material hydrotalcite, the mass ratio of the sodium lignosulfonate in the pulping aid is 30%, the mass percentage of the ethylhexyl phosphoric acid is 3%, the balance is polyethylene glycol, in the organic activation, the organic ammonium salt is dioctadecyl dimethyl ammonium chloride, the addition amount of the activation aid is preferably 1% of the mass of the raw material hydrotalcite, and the purification operation is as follows: adding 30% ethanol water solution with volume 3 times of the slurry in the step S1, stirring uniformly, standing for layering, removing supernatant, and repeating for 1-time.
Example 2
The preparation method of the modified hydrotalcite powder comprises the following steps:
step S1, coarsely selecting raw material hydrotalcite, crushing the hydrotalcite to a certain particle size, adding a certain amount of water and a pulping aid to prepare slurry, wherein the pulping aid is composed of ethylhexyl phosphoric acid, sodium dodecyl sulfate and polyethylene glycol with the molecular weight of 600;
step S2: purifying;
step S3: organic activation, adding a certain amount of organic ammonium salt and an activation aid, and carrying out activation reaction for a certain time, wherein the activation aid is 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride;
step S4: filtering, drying, crushing and sieving to obtain the modified hydrotalcite powder.
In the invention, the addition amount of a pulping aid is 8% of the mass of the raw material hydrotalcite, the mass ratio of sodium lignosulfonate in the pulping aid is 40%, the mass percentage of ethylhexyl phosphoric acid is 5%, the balance is polyethylene glycol, in organic activation, organic ammonium salt is dioctadecyl dihydroxyammonium chloride, the addition amount of the activation aid is 3% of the mass of the raw material hydrotalcite, and the purification operation is as follows: and (3) adding 20% ethanol aqueous solution which is 5 times of the volume of the slurry obtained in the step S1, uniformly stirring, standing for layering, removing supernate, and repeating for 3 times.
Example 3
The preparation method of the modified hydrotalcite powder comprises the following steps:
step S1, coarsely selecting raw material hydrotalcite, crushing the hydrotalcite to a certain particle size, adding a certain amount of water and a pulping aid to prepare slurry, wherein the pulping aid is composed of ethylhexyl phosphoric acid, sodium dodecyl sulfate and polyethylene glycol with molecular weight of 400;
step S2: purifying;
step S3: organic activation, adding a certain amount of organic ammonium salt and an activation aid, and carrying out activation reaction for a certain time, wherein the activation aid is 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride;
step S4: filtering, drying, crushing and sieving to obtain the modified hydrotalcite powder.
In the invention, the mass ratio of the sodium dodecyl sulfate in the pulping auxiliary agent is 35%, the mass percent of the ethylhexyl phosphate is 4%, the balance is polyethylene glycol, in the organic activation, the organic ammonium salt is dodecyl tertiary methyl hydrochloride, and the addition amount of the activation auxiliary agent is 2% of the mass of the raw material hydrotalcite. The purification operation is as follows: adding 25% ethanol water solution 4 times the volume of the slurry obtained in the step S1, stirring uniformly, standing for layering, removing supernatant, and repeating for 2 times.
Application example 1:
the novel calcium-zinc stabilizer for the PVC-U plate is prepared by processing the following components in parts by weight:
380 parts of zinc stearate, 90 parts of calcium stearate, 15 parts of soybean oil, 18 parts of activated calcium, 1 part of antioxidant, 12 parts of internal lubricant, 15 parts of external lubricant, 70 parts of modified hydrotalcite powder in example 1, 2 parts of β -copper and 40 parts of saxok.
Example 2
The novel calcium-zinc stabilizer for the PVC-U plate is prepared by processing the following components in parts by weight:
420 parts of zinc stearate, 100 parts of calcium stearate, 20 parts of soybean oil, 22 parts of activated calcium, 3 parts of an antioxidant, 16 parts of an internal lubricant, 20 parts of an external lubricant, 80 parts of modified hydrotalcite powder in example 2, 4 parts of β -copper and 60 parts of saxok.
Example 3
The novel calcium-zinc stabilizer for the PVC-U plate is prepared by processing the following components in parts by weight:
400 parts of zinc stearate, 96 parts of calcium stearate, 18 parts of soybean oil, 19.6 parts of activated calcium, 2 parts of antioxidant, 15 parts of internal lubricant, 18 parts of external lubricant, 75 parts of modified hydrotalcite powder in example 3, 3 parts of β -copper disulfide and 50 parts of mosaic.
Comparative example 1
The calcium-zinc stabilizer for the PVC-U sheet is prepared by processing the following components in parts by weight:
400 parts of zinc stearate, 96 parts of calcium stearate, 18 parts of soybean oil, 19.6 parts of activated calcium, 2 parts of antioxidant, 15 parts of internal lubricant, 18 parts of external lubricant, 75 parts of hydrotalcite powder (unmodified), 3 parts of β -copper and 50 parts of mosaic.
Comparative example 2
The calcium-zinc stabilizer for the PVC-U sheet is prepared by processing the following components in parts by weight:
400 parts of zinc stearate, 96 parts of calcium stearate, 18 parts of soybean oil, 19.6 parts of activated calcium, 2 parts of antioxidant, 15 parts of internal lubricant, 18 parts of external lubricant, 75 parts of modified hydrotalcite powder, 3 parts of β -copper disulfide and 50 parts of mosaic.
The preparation method of the modified hydrotalcite powder in comparative example 2 is as follows:
step S1, coarsely selecting raw material hydrotalcite, crushing the hydrotalcite to a certain particle size, adding a certain amount of water and a pulping aid to prepare slurry, wherein the pulping aid is composed of ethylhexyl phosphoric acid, sodium dodecyl sulfate and polyethylene glycol with molecular weight of 400;
step S2: purifying;
step S3: organic activation, adding a certain amount of organic ammonium salt, and carrying out activation reaction for a certain time;
step S4: filtering, drying, crushing and sieving to obtain the modified hydrotalcite powder.
In the invention, the mass ratio of the lauryl sodium sulfate in the pulping auxiliary agent is 35%, the mass percentage of the ethylhexyl phosphoric acid is 4%, the balance is polyethylene glycol, in the organic activation, the organic ammonium salt is dodecyl tertiary methyl hydrochloride, and the purification operation is as follows: adding 25% ethanol water solution 4 times the volume of the slurry obtained in the step S1, stirring uniformly, standing for layering, removing supernatant, and repeating for 2 times.
Comparative example 3
The calcium-zinc stabilizer for the PVC-U sheet is prepared by processing the following components in parts by weight:
400 parts of zinc stearate, 96 parts of calcium stearate, 18 parts of soybean oil, 19.6 parts of activated calcium, 2 parts of antioxidant, 15 parts of internal lubricant, 18 parts of external lubricant, 75 parts of modified hydrotalcite powder, 3 parts of β -copper (acetylacetone) and 50 parts of seik.
The preparation method of the modified hydrotalcite powder in the comparative example 3 is as follows:
step S1, coarsely selecting the raw material of hydrotalcite, crushing the hydrotalcite to a certain particle size, and adding a certain amount of water to prepare slurry;
step S2: purifying;
step S3: organic activation, adding a certain amount of organic ammonium salt and an activation aid, and carrying out activation reaction for a certain time, wherein the activation aid is 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride;
step S4: filtering, drying, crushing and sieving to obtain the modified hydrotalcite powder.
In the organic activation, the organic ammonium salt is dodecyl tertiary methyl hydrochloride, and the addition amount of the activation auxiliary agent is 2% of the mass of the raw material of the hydrotalcite. The purification operation is as follows: adding 25% ethanol water solution 4 times the volume of the slurry obtained in the step S1, stirring uniformly, standing for layering, removing supernatant, and repeating for 2 times.
Test examples
The calcium zinc stabilizers of examples 1-3 and comparative examples 1-3 and the commercially available general calcium zinc stabilizer are applied to processing of PVC-U plates, the addition amount is 4.3 parts, and the parts of other raw materials are as follows: 125 parts of PVC, 25 parts of calcium carbonate, 2.8 parts of titanium dioxide, 1.2 parts of ACR, 7.0 parts of CPE, mixing for 5-6 minutes, respectively carrying out rheometer detection on the mixed materials, processing the mixed materials into a PVC-U plate with the thickness of 25mm according to a conventional process, paying attention to the precipitation condition of a lubricating component in the processing process, and carrying out color difference detection on the plate. The results are as follows:
TABLE 1 results of mixture rheology test
TABLE 2 color difference test results for the panels
In conclusion, the calcium-zinc composite heat stabilizer is superior to the calcium-zinc heat stabilizer of the comparative example and the calcium-zinc heat stabilizer sold on the market, the processing torque of the mixture is smaller than that of the heat stabilizer of the comparative example and the heat stabilizer sold on the market, the performance meets the processing requirement of PVC-U plates, the color difference △ E, L, a and b values of the product are smaller than those of the comparative example, the appearance color difference is superior to that of the comparative example, in addition, the mixtures of the application examples 1-3 are found to have no obvious lubricating component precipitation in production, and the mixtures of the comparative example 2 and the calcium-zinc stabilizer sold on the market have obvious lubricating component precipitation and uneven plate.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (10)
1. The preparation method of the modified hydrotalcite powder is characterized by comprising the following steps:
step S1, coarsely selecting raw material hydrotalcite, crushing the hydrotalcite to a certain particle size, adding a certain amount of water and a pulping aid to prepare slurry, wherein the pulping aid is composed of ethylhexyl phosphoric acid, sodium dodecyl sulfate and polyethylene glycol with molecular weight of 200-600-;
step S2: purifying;
step S3: organic activation, adding a certain amount of organic ammonium salt and an activation aid, and carrying out activation reaction for a certain time, wherein the activation aid is 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride;
step S4: filtering, drying, crushing and sieving to obtain the modified hydrotalcite powder.
2. The preparation method of the modified hydrotalcite powder as claimed in claim 1, wherein the addition amount of the pulping assistant is 3-8% of the mass of the raw hydrotalcite, the mass ratio of the sodium dodecyl sulfate in the pulping assistant is 30-50%, the mass percentage of the ethylhexyl phosphoric acid is 3-8%, and the balance is polyethylene glycol.
3. The preparation method of the modified hydrotalcite powder as claimed in claim 2, wherein the addition amount of the pulping assistant is 5% of the mass of the raw hydrotalcite, the mass ratio of the sodium dodecyl sulfate in the pulping assistant is 30-40%, and the mass percentage of the ethylhexyl phosphoric acid is 3-5%.
4. The method for preparing modified hydrotalcite powder as claimed in claim 3, wherein the mass ratio of sodium dodecyl sulfate in the pulping assistant is 35%, and the mass percentage of ethylhexyl phosphoric acid is 4%.
5. The method for preparing modified hydrotalcite powder according to claim 1, wherein in the organic activation, the organic ammonium salt is one or a mixture of more of dioctadecyl dimethyl ammonium chloride, dioctadecyl dihydroxy ammonium chloride, octadecyl ammonium salt and dodecyl tertiary methyl hydrochloride.
6. The method for preparing modified hydrotalcite powder according to claim 1, wherein the addition amount of the activating assistant is 1-3% of the mass of the raw hydrotalcite.
7. The method for preparing modified hydrotalcite powder according to claim 6, wherein the addition amount of the activating assistant is 2% by mass of the raw hydrotalcite.
8. The method for preparing the modified hydrotalcite powder according to claim 1, wherein the purification operation is as follows: adding 20-30% ethanol aqueous solution with volume 3-5 times of the slurry in the step S1, stirring uniformly, standing for layering, removing supernatant, and repeating for 1-3 times.
9. Use of a modified hydrotalcite powder prepared by the process according to any one of claims 1 to 8 as a calcium zinc stabilizer.
10. The use of claim 9, wherein the calcium zinc stabilizer is any one of PVC-U sheet calcium zinc stabilizer, PVC pipe calcium zinc stabilizer, and PVC wire and cable calcium zinc stabilizer.
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| CN112063016A (en) * | 2020-11-16 | 2020-12-11 | 利安隆(天津)新材料科技有限公司 | Preparation method of long-acting phosphite ester antioxidant |
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| WO2007062671A1 (en) * | 2005-11-29 | 2007-06-07 | Pirelli Tyre S.P.A. | Tire and crosslinkable elastomeric composition |
| JP2007303025A (en) * | 2006-05-11 | 2007-11-22 | Kaisui Kagaku Kenkyusho:Kk | Polyurethane elastic fiber and dyeing auxiliary |
| JP2008001774A (en) * | 2006-06-21 | 2008-01-10 | Kaisui Kagaku Kenkyusho:Kk | Ultraviolet light absorber and its use |
| CN106700523A (en) * | 2016-12-21 | 2017-05-24 | 衢州普信新材料有限公司 | Preparation method of nano hydrotalcite composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007062671A1 (en) * | 2005-11-29 | 2007-06-07 | Pirelli Tyre S.P.A. | Tire and crosslinkable elastomeric composition |
| JP2007303025A (en) * | 2006-05-11 | 2007-11-22 | Kaisui Kagaku Kenkyusho:Kk | Polyurethane elastic fiber and dyeing auxiliary |
| JP2008001774A (en) * | 2006-06-21 | 2008-01-10 | Kaisui Kagaku Kenkyusho:Kk | Ultraviolet light absorber and its use |
| CN106700523A (en) * | 2016-12-21 | 2017-05-24 | 衢州普信新材料有限公司 | Preparation method of nano hydrotalcite composite material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112063016A (en) * | 2020-11-16 | 2020-12-11 | 利安隆(天津)新材料科技有限公司 | Preparation method of long-acting phosphite ester antioxidant |
| CN112063016B (en) * | 2020-11-16 | 2021-03-09 | 利安隆(天津)新材料科技有限公司 | Preparation method of long-acting phosphite ester antioxidant |
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