CN105271345B - A kind of preparation method of hard PVC special function filler super-fine active calcium carbide - Google Patents
A kind of preparation method of hard PVC special function filler super-fine active calcium carbide Download PDFInfo
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- CN105271345B CN105271345B CN201510680534.8A CN201510680534A CN105271345B CN 105271345 B CN105271345 B CN 105271345B CN 201510680534 A CN201510680534 A CN 201510680534A CN 105271345 B CN105271345 B CN 105271345B
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- stearic acid
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Abstract
A kind of preparation method of hard PVC special function filler super-fine active calcium carbide disclosed by the invention, is comprised the steps of：1) refined calcium hydroxide slurry is cooled to 30~32 DEG C, kiln gas is passed through after the chemical additives for adding two-component to be carbonized, control carburizing temperature to be less than 45 DEG C, carbonization was further continued for after the slurry pH value of carbonization reaches 7 10 minutes and obtained particle diameter is made in 190~210 nanometers of calcium carbonate superfine powder slurries；2) calcium carbonate superfine powder slurry is warming up to 70 DEG C, in the presence of high-shear emulsion machine, stearic acid and coconut oil compound coating agent saponification emulsion cladding processing 50~60 minutes are added, then carries out press filtration, drying, depolymerization and produces activation grade more than 99%, oil factor is less than 17g/100gCaCO3Hard PVC special function filler super-fine active calcium carbide product.
Description
Technical field
The present invention relates to a kind of preparation method of super-fine active calcium carbide, especially a kind of hard PVC special function filler
The preparation method of super-fine active calcium carbide.
Background technology
PVC is a kind of widely used general-purpose plastics, is, using Corvic as primary raw material, to add inserts and suitable
Age resister, modifying agent of amount etc., the material through techniques such as mixing, calendering, vacuum formings.PVC material have lightweight, every
The features such as heat, insulation, moistureproof, fire-retardant, easy construction, specification, color, pattern are various, are rich in dicoration, and its average consumption is only
Second is occupied inferior to polyethylene.
PVC can be divided into flexible PVC material and hard PVC material, and wherein hard PVC material constitutes about the 2/3 of market, soft
PVC material accounts for 1/3.In the production process of hard PVC section bar, in addition to adding appropriate auxiliary agent, in order to reduce production cost,
A large amount of inorganic particle calcium carbonate are usually added into, to improve dimensional stability, heat resistance, wearability and the rigidity of PVC profile, are improved
PVC plasticizing capacity.
Calcium carbonate is added in hard PVC section bar at present mainly has：(1) powdered whiting, it makes as the filler of increase-volume
With so as to reduce production cost.The inertia on powdered whiting surface, although carrying out stearic dry surface processing, due to place
Reason effect is poor, and with the increase of powdered whiting addition, the physicochemical property of PVC product significantly declines.(2) nano active carbon
Sour calcium, it is as the functional filler used in high-grade PVC product, except the heat resistance, wearability, size that can improve product are steady
Qualitative and rigidity etc. is outer, PVC product toughness reinforcing can also strengthened, any surface finish.But because the particle of nm-class active calcium carbonate is small, when
During loading increase, the viscosity increase of system, machine-shaping is difficult, therefore addition is also subject to certain restrictions.(3) lightweight is lived
Property calcium carbonate, the oil factor of the product is big, with the increase of loading, the viscosity of system increase, it is difficult to be molded, synthesis
Performance also declines.
The content of the invention：
The technical problem to be solved in the invention is to provide a kind of special low oil factor high filler loading capacity functional stuffing of hard PVC
The preparation method of super-fine active calcium carbide, briefly the particle diameter of the inserts is smaller than the particle diameter of powdered whiting, and nanometer is compared again
The particle diameter of calcium carbonate is big.Simultaneously simultaneous powdered whiting good fluidity, oil factor is low, and loading is big, has nano active carbon concurrently again
Sour calcium good surface activity, it is good with hard PVC compatibility, with significant activeness and quietness effect.
The technical problem solved required for of the invention, can be achieved through the following technical solutions：
A kind of preparation method of hard PVC special function filler super-fine active calcium carbide, it is characterised in that by following steps
Composition：
1) refined calcium hydroxide slurry is cooled to 30~32 DEG C, being passed through kiln gas after the chemical additives for adding two-component enters
Row carbonization, control carburizing temperature is less than 45 DEG C, carbonization was further continued for after the slurry pH value of carbonization reaches 7 10 minutes and system is made
Particle diameter is obtained in 190~210 nanometers of calcium carbonate superfine powder slurries；
2) calcium carbonate superfine powder slurry is warming up to 70 DEG C, in the presence of high-shear emulsion machine, adds stearic acid and coconut
Oily compound coating agent saponification emulsion cladding processing 50~60 minutes, then carry out press filtration, drying, depolymerization and produce activation grade and be more than
99%, oil factor is less than 17g/100gCaCO3Hard PVC special function filler super-fine active calcium carbide product.
In a preferred embodiment of the invention, in the step 1) in, the chemical additives of the two-component are added
Measure as 1.2~1.6wt% of weight of calcium carbonate in refined calcium hydroxide slurry.
In a preferred embodiment of the invention, in the step 1) in, the chemical additives of the two-component are sugarcane
The mixture of sugar and glucose, the wherein addition of sucrose and glucose is compared for 1 ﹕ 1.
In a preferred embodiment of the invention, in the step 2) in, stearic acid and the coconut oil compound coating
Agent saponification emulsion addition is 2.5~3.0wt% of weight of calcium carbonate in the calcium carbonate superfine powder slurry.
In a preferred embodiment of the invention, in the step 2) in, stearic acid and the coconut oil compound coating
The mass ratio of stearic acid and coconut oil is the ﹕ 1.4 of 1 ﹕ 0.6~1 in agent saponification emulsion.
In a preferred embodiment of the invention, in the step 2) in, stearic acid and the coconut oil compound coating
The preparation method of agent saponification emulsion is the stearic acid and coconut oil that formula ratio is added in 90 DEG C of hot water, then adds stearic acid
With 12~14wt% solid caustic soda of coconut oil total amount, saponification is dissolved into emulsion.
The advantage of the invention is that：
1st, in carbonisation, by adding two-component chemical additives, synthesize be adapted to hard PVC at a higher temperature
The calcium carbonate superfine powder particle of filler, reduces the energy consumption of low-temperature carbonization.
2nd, using compound coating agent, the covered effect of product is good, and oil factor is low, the good dispersion in hard PVC section bar, increases
Add loading, reduce the cost of manufacture of hard PVC section bar.
3rd, product of the present invention has coarse whiting good fluidity, and oil factor is low, and loading is big and nano-calcium carbonate good surface activity,
It is good with matrix compatibility, significantly increase the dual characteristicses of toughening effect.
Hard PVC functional stuffing super-fine active calcium carbide particle diameter prepared by the present invention is at 190~210 nanometers, and whiteness is more than
93, oil factor is less than 17, in polyvinyl chloride resin there is high filler loading capacity still to keep preferable combination property.
Embodiment
With reference to embodiment, the invention will be further described, but it is understood that these embodiments are not intended to limit this hair
Bright scope, in the case of without prejudice to spirit and scope of the invention, those skilled in the art can be to changes and improvements of the present invention
So that its different service conditions, condition and embodiment.
Embodiment 1
In 1 cubic metre of bubble type carburizing reagent kettle, add weight concentration and stood for 9.1% calcium hydroxide slurry 0.9
Square rice, adds sucrose and each 0.85 kilogram of lysate of glucose, is passed through CO2The concentration expressed in percentage by volume of gas is 28~31% kiln gas
It is carbonized, starting carburizing temperature is 31.6 DEG C, the flow for controlling kiln gas is 1.0 cubic metres per minute, is carbonized 10 minutes 1 hour
The pH value of disposed slurry is reduced to less than 7.0, and temperature is 44 DEG C, and it 10 minutes is carbonization terminal to be further continued for carbonization.
In the hot water that 1.4 kilograms of stearic acid and 1.6 kilograms of coconut oil are added to 20 kilograms 90 DEG C, and add 0.4 kilogram
Solid caustic soda carries out saponification.Then saponification emulsion is added and had warmed up into 70 DEG C of calcium carbonate slurry, and be stirred cladding processing 1
Hour.Slurries filtration after surface treatment to water content is finally less than to 40% filter cake, and in 80~110 DEG C of drying, depolymerization
Obtain product of the present invention.
The product measures particle diameter in 190~210 nanometers, soilless sticking phenomenon, whiteness 93.1, oil factor in TEM Electronic Speculum
16.8, hard PVC special function filler can be used as.
Embodiment 2
It is similar to Example 1,0.9 cubic metre of the calcium hydroxide slurry that weight concentration is 9.4% is added, sucrose and Portugal is added
Each 0.65 kilogram of lysate of grape sugar, is passed through CO2The concentration expressed in percentage by volume of gas is that 28~31% kiln gas are carbonized, starting carbonization
Temperature is 31.0 DEG C, and the flow for controlling kiln gas is 1.0 cubic metres per minute, and the pH value of 1 hour 15 minutes disposed slurry of carbonization is reduced to
Less than 7.0, temperature is 43 DEG C, and it 10 minutes is carbonization terminal to be further continued for carbonization.
In the hot water that 1.7 kilograms of stearic acid and 1.3 kilograms of coconut oil are added to 20 kilograms 90 DEG C, 0.42 kilogram is added
Solid caustic soda carries out saponification.Then saponification emulsion is added and had warmed up into 70 DEG C of calcium carbonate slurry, and be stirred cladding processing 1
Hour.Slurries filtration after surface treatment to water content is finally less than to 40% filter cake, and the depolymerization after 80~110 DEG C of drying
Obtain product of the present invention.
The product measures calcium carbonate particle diameter at 190~200 nanometers in TEM Electronic Speculum, and soilless sticking phenomenon, whiteness 93.5 is inhaled
Oily value 16.3, can be used as hard PVC special function filler.
Reference examples 1
Method similar to Example 1, adds 0.9 cubic metre of the calcium hydroxide slurry that weight concentration is 9.1%, adds sugarcane
Sugared 1.7 kilograms of lysates, are passed through CO2The concentration expressed in percentage by volume of gas is that 28~31% kiln gas are carbonized, and originates carburizing temperature
For 30.2 DEG C, control kiln gas flow be 1.0 cubic metres per minute, carbonization 1 hour 10 minutes disposed slurry pH value be reduced to 7.0 with
Under, the outlet temperature of carbonization is 35 DEG C, and it 10 minutes is carbonization terminal to be further continued for carbonization.
In the hot water that 3.0 kilograms of stearic acid is added to 20 kilograms 90 DEG C, add 0.4 kilogram of solid caustic soda and carry out saponification.Then
Saponification emulsion is added and had warmed up into 70 DEG C of calcium carbonate slurry, and is stirred cladding processing 1 hour.Finally by surface
Slurries filtration after reason is less than 40% filter cake to water content, and depolymerization obtains product after 80~110 DEG C of drying.
The product measures calcium carbonate particle diameter at 70~90 nanometers in TEM Electronic Speculum, slightly agglomeration, whiteness 93.1, inhales
Oily value 22.8, when filling hard PVC resin processing procedure, fluidity is poor, is unfavorable for processing.
General principle, principal character and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, various changes and modifications of the present invention are possible without departing from the spirit and scope of the present invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.
Claims (1)
1. a kind of preparation method of hard PVC special function filler super-fine active calcium carbide, it is characterised in that by following steps group
Into：
1) refined calcium hydroxide slurry is cooled to 31~31.6 DEG C, kiln gas progress is passed through after the chemical additives for adding two-component
Carbonization, it is 43~44 DEG C to control carburizing temperature, carbonization was further continued for after the slurry pH value of carbonization reaches 7 10 minutes and grain is made
Footpath is in 190~210 nanometers of calcium carbonate superfine powder slurries；
2) calcium carbonate superfine powder slurry is warming up to 70 DEG C, in the presence of high-shear emulsion machine, adds stearic acid and coconut oil is multiple
Close covering saponification emulsion cladding processing 50~60 minutes, then carry out press filtration, drying, depolymerization and produce activation grade more than 99%, inhale
Oil value is less than 17g/100gCaCO3Hard PVC special function filler super-fine active calcium carbide product；
In the step 1) in, the chemical additives addition of the two-component is calcium hydroxide weight in refined calcium hydroxide slurry
1.2~1.6wt% of amount；
In the step 1) in, the chemical additives of the two-component are sucrose and the mixture of glucose, wherein sucrose and Portugal
The mass ratio of grape sugar is 1 ﹕ 1；
In the step 2) in, stearic acid and coconut oil compound coating agent saponification the emulsion addition is the calcium carbonate superfine powder
2.5~3.0wt% of weight of calcium carbonate in slurry；
In the step 2) in, the quality of stearic acid and coconut oil in stearic acid and coconut oil compound coating the agent saponification emulsion
Than for the ﹕ 1.4 of 1 ﹕ 0.6~1；
In the step 2) in, the preparation method of stearic acid and coconut oil compound coating the agent saponification emulsion is the heat at 90 DEG C
The stearic acid and coconut oil of formula ratio are added in water, stearic acid and 12~14wt% solid caustic soda of coconut oil total amount, soap is then added
Change is dissolved into emulsion.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105694291A (en) * | 2016-03-17 | 2016-06-22 | 海南联塑科技实业有限公司 | Cold-resistant polyvinyl chloride pipeline and preparation method thereof |
| CN109399683B (en) * | 2018-12-06 | 2020-12-01 | 东北大学 | Preparation method of nano calcium carbonate for yield enhancement of PVC (polyvinyl chloride) automobile primer |
| CN109399682A (en) * | 2018-12-06 | 2019-03-01 | 河南省科学院高新技术研究中心 | A kind of food additives active nano-calcium carbonate and preparation method thereof |
| CN112079374A (en) * | 2020-09-22 | 2020-12-15 | 江西省科学院能源研究所 | Preparation method of nano-grade active calcium carbonate for plastic film |
| CN113061353A (en) * | 2021-03-26 | 2021-07-02 | 上海南卓新材料科技有限公司 | Preparation method of filling calcium carbonate for offset printing rotary press ink and product thereof |
| CN113060751B (en) * | 2021-03-26 | 2023-04-18 | 上海南卓新材料科技有限公司 | Preparation method of nano calcium carbonate filler for LED-UV ink and product |
| CN117624853B (en) * | 2024-01-23 | 2024-04-05 | 天津永续新材料有限公司 | Bamboo powder modified polylactic acid-based biodegradable composite material and preparation method thereof |
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| CN1211286C (en) * | 2001-08-03 | 2005-07-20 | 上海华明高技术（集团）有限公司 | Industrial process for preparing nm-class active calcium carbonate |
| CN101531391B (en) * | 2009-04-16 | 2011-05-18 | 芜湖卓越纳米新材料有限公司 | Method for industrially preparing nanometer calcium carbonate for solvent type ink addition agent |
| CN101570342B (en) * | 2009-06-11 | 2011-08-24 | 福建省万旗非金属材料有限公司 | Method for preparing high-whiteness nanometer calcium carbonate special for silicone sealant by utilizing low-grade limestone by wet method |
| CN101774623B (en) * | 2010-01-19 | 2012-09-26 | 上海卓越纳米新材料股份有限公司 | Industrial preparation method of rice-shaped ultra-fine activated calcium carbonate |
| CN103818941A (en) * | 2013-05-27 | 2014-05-28 | 芜湖卓越纳米新材料有限公司 | Preparation method of special low-viscosity activated calcium carbonate for silicone adhesive |
| CN103754914B (en) * | 2013-12-04 | 2015-08-05 | 芜湖卓越纳米新材料有限公司 | The preparation method of the special low oil-absorption(number) submicron activated Calcium carbonate of a kind of PVC |
| CN103738993B (en) * | 2013-12-04 | 2015-11-04 | 芜湖卓越纳米新材料有限公司 | A kind of carbonization reactor of energy-saving nano-calcium carbonate and preparation method |
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