CN105331010A - Preparation method of PVC resin filler - Google Patents
Preparation method of PVC resin filler Download PDFInfo
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- CN105331010A CN105331010A CN201510846126.5A CN201510846126A CN105331010A CN 105331010 A CN105331010 A CN 105331010A CN 201510846126 A CN201510846126 A CN 201510846126A CN 105331010 A CN105331010 A CN 105331010A
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- calcium carbonate
- weighting agent
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- chloride resin
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Abstract
The invention relates to a preparation method of CPVC resin filler, which is a method for preparing the PVC resin filler by taking ardealite as a raw material. The preparation method of the PVC resin filler comprises the steps of reacting the ardealite subjected to edulcoration with sodium carbonate to obtain calcium carbonate; performing anaerobic fermentation on the obtained calcium carbonate, candy pomace and bean dregs under the action of lactic acid bacteria to obtain lactic acid; performing esterification reaction on the obtained lactic acid and stearic acid under the action of protective gas, and performing neutralization reaction on stearic acid lactoyl acid and calcium carbonate which are generated by reaction, thus obtaining calcium lactate stearate. The obtained calcium lactate stearate is taken as filler for the production of PVC resin. The preparation method solves the environment pollution problem of the ardealite, reduces treatment charges paid by an enterprise for solving the problem, and has very obvious economic practicality.
Description
Technical field
The present invention relates to a kind of preparation method of polyvinyl chloride resin weighting agent, is take phosphogypsum as the method for waste polyvinyl chloride resin weighting agent.
Background technology
Show according to relevant statistics, at present, China every year newly-increased phosphogypsum quantity discharged reaches 5,000 ten thousand tons, a large amount of phosphogypsums is stacked, not only land occupation resource, increase tremendous economic burden to enterprise, but also certain pollution can be caused to environment, cause huge pressure to the development of the national economy of China and ecotope.Therefore, accelerate the comprehensive utilization technique creativity of phosphogypsum, realize turning waste into wealth, turning bane into boon, having become in China's economic construction an important techno-economic policy, is also the problem in the urgent need to address of Faced In Sustainable Development.According to the gist of a document of " State Council is about the notice printing and distributing Circular Economy Development Strategy and Immediate action plan " (No. [2013] 5, promulgated by the State Council), one of resource utilization major construction projects have been listed in the comprehensive utilization of the industrial solid castoff such as phosphogypsum, flyash in, become Establishing Circular Economy Syste m in China, one of vital task of building a resource-conserving and environment-friendly society.
Current phosphogypsum is widely used preparing the building field such as cement setting retarder, building materials of gypsum.But manufacture field at polyvinyl chloride resin, utilizing of phosphogypsum is few, significantly limit the recycling of phosphogypsum, and therefore needing provides a kind of innovative technology to solve the problem, to widen the range of application of phosphogypsum.
Summary of the invention
For the limitation that existing phosphogypsum is applied, the object of the present invention is to provide a kind of preparation method of polyvinyl chloride resin weighting agent, to expand phosphogypsum range of application.
The present invention adopts following technical scheme: a kind of preparation method of polyvinyl chloride resin weighting agent, said method comprising the steps of:
1) obtained calcium carbonate is reacted through the phosphogypsum of removal of impurities process and sodium carbonate;
2) step 1) calcium carbonate of gained and sugared slag, bean dregs anaerobically fermenting under milk-acid bacteria effect obtain lactic acid;
3) step 2) lactic acid of gained, stearic acid carry out esterification, the lactylates acid that reaction generates and step 1 under shielding gas effect) calcium carbonate of gained carries out neutralization reaction and obtains CSL weighting agent.
Preferably: the weight percentage of phosphogypsum impurity described 1) is less than 5%.
Sugared slag preferably: step 2) is the by product after sugarcane carries sugar, and in massfraction, sugared slag sugar degree is 35 ~ 42%, and the byproduct in soymilk or bean curd process produced by described bean dregs, and in massfraction, bean dregs are containing 10 ~ 20% protein.
Calcium carbonate preferably: step 2), sugared slag, bean dregs weight ratio are 0.3:2:1 ~ 0.5:3:2.
The temperature of anaerobically fermenting preferably: step 2) is 35 ~ 40 DEG C, and the anaerobically fermenting time is 24 ~ 48 hours.
Lactic acid preferably: step 3) and stearic acid are pressed 2:1 ~ 3:1 mol ratio and are added.
The mol ratio of calcium carbonate preferably: step 3) and lactic acid two material is 1:2 ~ 1:3.
Shielding gas preferably: step 3) is nitrogen.
The method preparing polyvinyl chloride resin weighting agent provided by the invention has following characteristics:
1, the CSL obtained by the present invention can be used as tensio-active agent and is applied to polyvinyl chloride resin production.CSL has hydrophilic polar and hydrophobic apolar two kinds of groups.CSL is by the polar molecule surface of the hydrophilic radical oriented adsorption in molecule at the inorganic filler such as tinting material, extender, then oriented adsorption is surperficial at PVC molecular layer for its hydrophobic grouping, improve the dispersiveness of each weighting agent in PVC base-material and wettability, thus the avidity improved between various weighting agent and PVC, make the polyvinyl chloride resin performance prepared more stable, outward appearance, color and luster are fuller.
2, the main component of phosphogypsum of the present invention is calcium sulfate, utilizes reaction equation:
Na
2CO
3+CaSO
4＝Na
2SO
4+CaCO
3
Make it to be converted into calcium carbonate, then prepare CSL further, using the CSL of gained as one of PVC weighting agent, solve the pollution problem of phosphogypsum to environment, reduce the processing costs that enterprise pays for it, there is fairly obvious economic and practical.
3, sugared slag is the by product after sugarcane carries sugar, containing moisture, the organic substances such as residual sugar, fiber, amino acid, the byproduct in soymilk or bean curd process produced by bean dregs, containing organic matters such as moisture, protein, fat, carbohydrate (Mierocrystalline cellulose, polysaccharide etc.), these two kinds of materials are all applicable to the growth of spoilage microorganisms, very easily cause the waste of resource and the pollution of environment.The present invention utilizes sugared slag, lactic acid prepared by bean dregs, solves sugared slag, bean dregs to the pollution problem of environment, reduces the cost of farming industry process waste and make it resource utilization, make enterprise change profit evaluation model environmental protection into by feeding type environmental protection.
4, intermediates of the present invention utilize as calcium carbonate, calcium lactate all can be used as PVC weighting agent, and described lactic acid can be obtained by lactic acid and calcium carbonate reaction.Greatly improve the utilization ratio of each intermediate product, reduce the treatment step of newborn substance.
Embodiment
Further describe technical scheme of the present invention below, but described in claimed scope is not limited to.Below in conjunction with specific embodiment, elaboration detailed is further done to the present invention, but embodiments of the present invention are not limited to the scope that embodiment represents.These embodiments only for illustration of the present invention, but not for limiting the scope of the invention.In addition, after reading content of the present invention, those skilled in the art can do various amendment to the present invention, and these equivalent variations fall within appended claims limited range of the present invention equally.
Embodiment 1
Removal of impurities process is carried out to phosphogypsum, the impurity weight percentage contained by phosphogypsum is controlled to be 4%.Phosphogypsum and excess of sodium carbonate are reacted, filtration, washing, dry obtained calcium carbonate.After calcium carbonate, sugarcane are carried sugar, the by product sugar slag of gained, the bean dregs of production soymilk gained are placed in fermenting container by 0.3:2:1 mass ratio, add milk-acid bacteria, stir, anaerobically fermenting 48 hours at 35 DEG C, obtained lactic acid after separating-purifying in fermenting container; Described viable count of lactobacillus by every gram of sugared slag containing 4,000,000; In massfraction, sugared slag sugar degree is 35%; In massfraction, bean dregs are containing 10% protein.The lactic acid of gained and stearic acid are pressed in the three-necked bottle that 2:1 mixed in molar ratio loads with agitator, add winterized stearin as catalyzer, pass into nitrogen, rapid temperature increases to 180 DEG C under agitation condition also keeps 40min, the acid of lactate synthesis lactylates.After esterification completes, add calcium carbonate (mol ratio of described calcium carbonate and lactic acid two material is 1:2), stirring reaction 40min, by reactor cooling to normal temperature.Products obtained therefrom is dissolved in water, filters, wash and can obtain CSL.The CSL of gained mixed with thermo-stabilizer, toughner, lubricant, tinting material, PVC, through extruding, the technique such as sizing obtains polyvinyl chloride resin.
Embodiment 2
Removal of impurities process is carried out to phosphogypsum, the impurity weight percentage contained by phosphogypsum is controlled to be 3%.Phosphogypsum and excess of sodium carbonate are reacted, filtration, washing, dry obtained calcium carbonate.After calcium carbonate, sugarcane are carried sugar, the by product sugar slag of gained, the bean dregs of production bean curd gained are placed in fermenting container by 0.4:2.5:1.5 mass ratio, milk-acid bacteria is added in fermenting container, stir, anaerobically fermenting 36 hours at 38 DEG C, obtained lactic acid after separating-purifying; Described viable count of lactobacillus by every gram of sugared slag containing 4,500,000; In massfraction, sugared slag sugar degree is 37%; In massfraction, bean dregs are containing 15% protein.The lactic acid of gained and stearic acid are pressed in the three-necked bottle that 2.5:1 mixed in molar ratio loads with agitator, add winterized stearin as catalyzer, pass into nitrogen, rapid temperature increases to 200 DEG C under agitation condition also keeps 35min, the acid of lactate synthesis lactylates.After esterification completes, add calcium carbonate (mol ratio of described calcium carbonate and lactic acid two material is 1:2.5), stirring reaction 30min, by reactor cooling to normal temperature.Products obtained therefrom is dissolved in water, filters, wash and can obtain CSL.CSL, calcium carbonate are mixed with thermo-stabilizer, toughner, lubricant, tinting material, PVC, through extruding, the technique such as sizing obtains polyvinyl chloride resin.
Embodiment 3
Removal of impurities process is carried out to phosphogypsum, the impurity weight percentage contained by phosphogypsum is controlled to be 2%.Phosphogypsum and excess of sodium carbonate are reacted, filtration, washing, dry obtained calcium carbonate.After calcium carbonate, sugarcane are carried sugar, the by product sugar slag of gained, the bean dregs of production bean curd gained are placed in fermenting container by 0.5:3:2 mass ratio, add milk-acid bacteria, stir, anaerobically fermenting 24 hours at 40 DEG C, obtained lactic acid after separating-purifying in fermenting container; Described viable count of lactobacillus by every gram of sugared slag containing 5,000,000; In massfraction, sugared slag sugar degree is 42%; In massfraction, bean dregs are containing 20% protein.The lactic acid of gained and stearic acid are pressed in the three-necked bottle that 3:1 mixed in molar ratio loads with agitator, add winterized stearin as catalyzer, pass into nitrogen, rapid temperature increases to 210 DEG C under agitation condition also keeps 28min, the acid of lactate synthesis lactylates.After esterification completes, add calcium carbonate (mol ratio of described calcium carbonate and lactic acid two material is 1:3), stirring reaction 30min, by reactor cooling to normal temperature.Products obtained therefrom is dissolved in water, filters, wash and can obtain CSL.CSL, calcium carbonate, calcium lactate (calcium carbonate and lactic acid reaction product) are mixed with thermo-stabilizer, toughner, lubricant, tinting material, PVC, through extruding, the technique such as sizing obtains polyvinyl chloride resin.
Claims (8)
1. a preparation method for polyvinyl chloride resin weighting agent, is characterized in that, said method comprising the steps of:
1) obtained calcium carbonate is reacted through the phosphogypsum of removal of impurities process and sodium carbonate;
2) step 1) calcium carbonate of gained and sugared slag, bean dregs anaerobically fermenting under milk-acid bacteria effect obtain lactic acid;
3) step 2) lactic acid of gained, stearic acid carry out esterification, the lactylates acid that reaction generates and step 1 under shielding gas effect) calcium carbonate of gained carries out neutralization reaction and obtains CSL weighting agent.
2. the preparation method of polyvinyl chloride resin weighting agent according to claim 1, is characterized in that, described 1), phosphogypsum impurity weight percentage is less than 5%.
3. the preparation method of polyvinyl chloride resin weighting agent according to claim 1, it is characterized in that, step 2) described in sugared slag be by product after sugarcane carries sugar, in massfraction, sugar slag sugar degree is 35 ~ 42%, the byproduct in soymilk or bean curd process produced by described bean dregs, and in massfraction, bean dregs are containing 10 ~ 20% protein.
4. the preparation method of the polyvinyl chloride resin weighting agent according to claim 1 or 3, is characterized in that, step 2) described in calcium carbonate, sugared slag, bean dregs weight ratio be 0.3:2:1 ~ 0.5:3:2.
5. the preparation method of polyvinyl chloride resin weighting agent according to claim 1, is characterized in that, step 2) described in the temperature of anaerobically fermenting be 35 ~ 40 DEG C, the anaerobically fermenting time is 24 ~ 48 hours.
6. the preparation method of polyvinyl chloride resin weighting agent according to claim 1, is characterized in that, step 3) described in lactic acid and stearic acid press 2:1 ~ 3:1 mol ratio and add.
7. the preparation method of polyvinyl chloride resin weighting agent according to claim 1, is characterized in that, step 3) described in the mol ratio of calcium carbonate and lactic acid two material be 1:2 ~ 1:3.
8., according to the preparation method of described polyvinyl chloride resin weighting agent arbitrary in claim 1,6,7, it is characterized in that, step 3) described in shielding gas be nitrogen.
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| CN201510846126.5A CN105331010A (en) | 2015-11-29 | 2015-11-29 | Preparation method of PVC resin filler |
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| CN201510846126.5A CN105331010A (en) | 2015-11-29 | 2015-11-29 | Preparation method of PVC resin filler |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105802067A (en) * | 2016-04-07 | 2016-07-27 | 广州煌垅生物科技有限公司 | Safe and environment-friendly heat stabilizer for PVC (polyvinyl chloride) plastics and preparation method of heat stabilizer |
| CN107573565A (en) * | 2017-09-13 | 2018-01-12 | 苏州南诚塑料制品有限公司 | A kind of soft plastic formula and preparation technology |
| CN112322066A (en) * | 2020-11-22 | 2021-02-05 | 邵阳天堂助剂化工有限公司 | Modified bean dreg-based environment-friendly composite heat stabilizer for PVC (polyvinyl chloride) |
| CN112521701A (en) * | 2020-12-17 | 2021-03-19 | 淄博盘广塑胶有限公司 | PVC filler |
Citations (2)
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| CN102220388A (en) * | 2010-04-15 | 2011-10-19 | 中国科学院过程工程研究所 | Method for clean production of lactic acid by calcium salt process |
| CN102517346A (en) * | 2011-12-16 | 2012-06-27 | 安徽中粮生化格拉特乳酸有限公司 | Method for preparing L-lactic acid and/or L-lactate |
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2015
- 2015-11-29 CN CN201510846126.5A patent/CN105331010A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220388A (en) * | 2010-04-15 | 2011-10-19 | 中国科学院过程工程研究所 | Method for clean production of lactic acid by calcium salt process |
| CN102517346A (en) * | 2011-12-16 | 2012-06-27 | 安徽中粮生化格拉特乳酸有限公司 | Method for preparing L-lactic acid and/or L-lactate |
Non-Patent Citations (1)
| Title |
|---|
| 张亚丽: ""硬脂酰乳酸钙的制备工艺研究"", 《食品工业科技》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105802067A (en) * | 2016-04-07 | 2016-07-27 | 广州煌垅生物科技有限公司 | Safe and environment-friendly heat stabilizer for PVC (polyvinyl chloride) plastics and preparation method of heat stabilizer |
| CN107573565A (en) * | 2017-09-13 | 2018-01-12 | 苏州南诚塑料制品有限公司 | A kind of soft plastic formula and preparation technology |
| CN112322066A (en) * | 2020-11-22 | 2021-02-05 | 邵阳天堂助剂化工有限公司 | Modified bean dreg-based environment-friendly composite heat stabilizer for PVC (polyvinyl chloride) |
| CN112322066B (en) * | 2020-11-22 | 2022-08-30 | 湖南雄创新材料科技有限公司 | Modified bean dreg environment-friendly composite heat stabilizer for PVC |
| CN112521701A (en) * | 2020-12-17 | 2021-03-19 | 淄博盘广塑胶有限公司 | PVC filler |
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Application publication date: 20160217 |