CN114773749B - Low-voc polyvinyl chloride plastic material and preparation method thereof - Google Patents
Low-voc polyvinyl chloride plastic material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/22—After-treatment of expandable particles; Forming foamed products
- C08J9/228—Forming foamed products
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B13/00—Conditioning or physical treatment of the material to be shaped
- B29B13/10—Conditioning or physical treatment of the material to be shaped by grinding, e.g. by triturating; by sieving; by filtering
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
- C08J9/0071—Nanosized fillers, i.e. having at least one dimension below 100 nanometers
- C08J9/008—Nanoparticles
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2497/00—Characterised by the use of lignin-containing materials
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Abstract
The invention discloses a low-voc polyvinyl chloride plastic material and a preparation method thereof, belonging to the technical field of modified plastics. The low-voc polyvinyl chloride plastic material of the invention comprises the following components: porous polyvinyl chloride particles, nano TiO2, cellulose nanocrystals, sodium lignin sulfonate, rubber wear-resistant agents, calcium stearate, polyol wax, phosphate antioxidants and calcined kaolin. The invention selects porous polyvinyl chloride particles and selects nano TiO aiming at the adaptability of the porous polyvinyl chloride particles 2 The cellulose nanocrystals and the sodium lignin sulfonate are compounded to serve as the voc inhibitor, and the release amount of the voc can be obviously reduced through ball milling treatment, so that the environmental protection performance is improved, and the method has a good application prospect.
Description
Technical Field
The invention belongs to the technical field of modified plastics, and particularly relates to a low-voc polyvinyl chloride plastic material and a preparation method thereof.
Background
The plastic material is a material for producing plastic products, which is mainly prepared by taking polymer synthetic resin as a raw material, adding various auxiliary materials and additives in production engineering, and melting the auxiliary materials and the additives into the polymer synthetic resin to form a material which has plasticity and fluidity at a specific temperature and under a specific pressure, can be molded into a certain shape and keeps the shape unchanged under a certain condition. The polymer synthetic resin raw materials are mostly PE, PP, PVC, ABS and the like, the produced plastic material is used for manufacturing plastic, and the plastic has very wide application and is an indispensable component in household appliances, automobiles, mobile phones, PCs, medical appliances and lighting appliances. With the rapid development of the plastic industry and the continuous improvement of plastic performance, plastic products are widely applied, the plastic products are replacing traditional metal parts in different fields, and a reasonably designed plastic part can often replace a plurality of traditional metal parts, so that the development and production of novel plastic with excellent characteristics have good development prospect.
At present, the plastic materials still have the following defects: most of traditional plastic products contain a certain amount of volatile organic compounds (voc for short), and because the plastic products are widely applied to various household products, in the process of storing the plastic products in a relatively closed living room, the voc is volatilized continuously, when the voc in the living room reaches a certain concentration, people feel headache, nausea, vomiting, hypodynamia and the like in a short time, and in severe cases, convulsions and coma occur, and the liver, the kidney, the brain and the nervous system of the people are injured, so that serious consequences such as hypomnesis and the like are caused.
The Chinese patent application CN201410175746.6 is a low-phenol environment-friendly floor tile, which comprises, by mass, 100 parts of polyvinyl chloride resin, 25-35 parts of dioctyl terephthalate, 2-3 parts of epoxidized soybean oil, 2-3 parts of powder calcium-zinc composite stabilizer, 0.5-1 part of benzophenone ultraviolet light absorber and 4-10 parts of phosphate flame retardant, and has the low-phenol standard of European Union, the low-VOC release standard of European Union interior decoration materials and the limit standard of harmful substances in the polyvinyl chloride coiled material floor of GB18586-2001 interior decoration materials. In the patent, after all raw materials are metered, the raw materials are mixed at a low speed for 10 seconds and then mixed at a high speed for 4 minutes, and the raw materials are fully mixed under high-speed stirring to obtain a mixture, and then extrusion molding is carried out. The reduction in voc release is relatively limited.
Therefore, there is an urgent need for a plastic material with lower voc to better adapt to the application requirements, environmental protection requirements, etc. of the plastic material in the closed space of furniture and the like.
Disclosure of Invention
The invention aims to provide a low-voc polyvinyl chloride plastic material and a preparation method thereof, which are characterized in that porous polyvinyl chloride (PVC) particles are utilized, and in combination with a voc inhibitor with better applicability, the release of voc is greatly reduced, and the safety and environmental protection of the material are improved.
In order to achieve the above object, the present invention has the following technical scheme:
firstly, the invention provides a low-voc polyvinyl chloride plastic material, which comprises the following components:
porous polyvinyl chloride particles and nano TiO 2 Cellulose nanocrystals, sodium lignin sulfonate, rubber antiwear agents, calcium stearate, polyol wax, phosphate antioxidants, calcined kaolin.
Preferably, the porous polyvinyl chloride particles have a porosity of 60-80%.
Preferably, the pore size of the porous polyvinyl chloride particles is 10-1000nm.
Preferably, the D50 particle size of the nano titanium dioxide is 5-50nm, and the D90 particle size is 10-100nm.
Preferably, the low voc polyvinyl chloride plastic material comprises the following components in parts by weight:
100 parts of porous polyvinyl chloride particles and nano TiO 2 1-15 parts of cellulose nanocrystals, 1-10 parts of sodium lignin sulfonate, 0.2-4 parts of rubber wear-resistant agent, 1-5 parts of calcium stearate, 0.05-0.5 part of polyol wax, 0.5-3 parts of phosphate antioxidant and 10-15 parts of calcined kaolin.
Further preferably, porous polyvinyl chloride particles, nano TiO 2 The mass ratio of cellulose nanocrystals to sodium lignin sulfonate is controlled at 20:2:1:0.1.
most preferably, the low voc polyvinyl chloride plastic compound comprises the following components in parts by weight:
100 parts of porous polyvinyl chloride particles and nano TiO 2 10 parts of cellulose nanocrystals, 0.5 part of sodium lignin sulfonate, 2 parts of rubber wear-resistant agent, 0.1 part of calcium stearate, 1 part of polyol wax, 0.04 part of phosphate antioxidant and 15 parts of calcined kaolin.
Secondly, the invention provides a preparation method of the low-voc polyvinyl chloride plastic material, which comprises the following steps:
(1) Porous polyvinyl chloride particles and nano TiO 2 Fully mixing cellulose nanocrystals and sodium lignin sulfonate, and performing ball milling treatment to obtain a mixture 1;
(2) And (3) fully mixing the mixture 1, the rubber wear-resistant agent, calcium stearate, polyol wax, phosphate antioxidant and calcined kaolin, adding the mixture into a double-screw extruder, and extruding to obtain the low-voc polyvinyl chloride plastic material.
Preferably, the mixing in steps (1) and (2) is carried out by a V-shaped particle mixer.
Preferably, in the step (1), the ball milling treatment conditions are as follows: the rotating speed is 100-1000r/min, and the ball-material ratio is 5-20:1, ball milling time is 5-20min.
Further preferably, in step (1), the ball milling treatment conditions are: the rotating speed is 450r/min, and the ball-material ratio is 10:1, ball milling time is 15min.
Preferably, in the step (2), the temperature of the front section in the twin-screw extruder is kept at 160-170 ℃, the temperature of the middle section is kept at 160-165 ℃, the temperature of the rear section is kept at 140-150 ℃, the color yellowing caused by the long-time heated degradation of PVC and the suction of hydrogen chloride is prevented, and the transparency of the product is ensured.
The beneficial effects of the invention are as follows:
(1) The invention creatively selects the porous polyvinyl chloride particles and selects the nano TiO aiming at the adaptability of the porous polyvinyl chloride particles 2 The cellulose nanocrystals and the sodium lignin sulfonate are compounded to serve as the voc inhibitor, and the release amount of the voc can be obviously reduced through ball milling treatment, so that the environmental protection performance is improved, and the method has a good application prospect.
(2) The selected raw materials are environment-friendly, wide in sources, simple in preparation method and easy to produce, and meanwhile, the produced low-voc polyvinyl chloride plastic material is good in transparency and high in value.
Detailed Description
In order to make the technical means, the creation features, the achievement of the purpose and the effect of the present invention easy to understand, the present invention will be further elucidated with reference to the specific embodiments, but the following embodiments are only preferred embodiments of the present invention, not all of them. Based on the examples in the embodiments, those skilled in the art can obtain other examples without making any inventive effort, which fall within the scope of the invention. In the following examples, unless otherwise specified, the methods of operation used were conventional, the equipment used was conventional, and the materials used in the examples were the same.
In the following examples, nano TiO 2 Purchased from guangzhou radium liter science and technology company under the model LS511, d50=10nm, d90=80 nm; cellulose nanocrystals were purchased from Gui Linji macro technology under the trade designation C-CNC; sodium lignin sulfonate was purchased from the Guangzhou Ying Xiang chemical Co., ltd; rubber antiwear agent is purchased from Guangzhou Longkai chemical industry with the product number KH-Si69 (bis- [3- (triethoxysilyl) propyl)]Tetrasulfide); polyol wax was purchased from germany as Mu Li under the trade designation Loxiol GH4; phosphate antioxidants were purchased from basf under the product number 168; calcined kaolin was purchased from the Guangzhou Zhengfei chemical industry under the product number 1250; the model of the double-screw extruder is SMD-65, and the Dongguan city Sanyou plastic machinery manufacturing company; the model of the V-shaped particle mixer is 200L, and Shenzhen Henghao Xiang technology Co., ltd.
1. Preparation of porous polyvinyl chloride particles
(1) Adding polyvinyl chloride powder into cyclohexanone (the volume mass ratio of the cyclohexanone to the polyvinyl chloride powder is 10:1), heating in a water bath to 50 ℃, preserving heat and stirring until the polyvinyl chloride is completely dissolved, adding a pore-forming agent potassium chloride (the mass ratio of the potassium chloride to the polyvinyl chloride powder is 8:1), and stirring uniformly to obtain injection;
(2) Dripping the injection liquid obtained in the step (1) into distilled water, rapidly stirring while dripping, filtering, washing, removing pore-forming agent, and drying to obtain porous polyvinyl chloride particles A.
The porous polyvinyl chloride particles B, C, D with different porosities and pore diameters are prepared by adjusting the volume-mass ratio of cyclohexanone to polyvinyl chloride powder, the mass ratio of potassium chloride to polyvinyl chloride powder and the stirring rotation speed, and the characterization results of the porous polyvinyl chloride particles A, B, C, D are as follows:
| A | B | C | D | |
| particle size distribution | 0.5-8mm | 0.5-8mm | 0.5-8mm | 0.5-8mm |
| Porosity of the porous material | 72％ | 63％ | 77％ | 98％ |
| Average pore diameter | 234nm | 261nm | 196nm | 205nm |
2. Preparation of low-voc polyvinyl chloride plastic material
Examples 1 to 3
The low voc polyvinyl chloride molding compound was prepared according to the following procedure.
Machine cleaning:
mixing 50g of screw cleaner and 1.5kg of porous PVC particles to form a cleaning material, pouring the mixed cleaning material into a hopper of a double-screw plastic extruding machine, emptying the glue for about half a minute by using sol, cleaning the hopper by using cloth after the cleaning material is injected, adding a quantity of sizing materials for an injection molding machine, cleaning the cleaning material stored on a screw, repeatedly putting the discharged cleaning material into the hopper for 2-3 times, fully cleaning, controlling the temperature of the screw of the double-screw plastic extruding machine within 200 ℃ in the cleaning process, and arranging a dry hopper at the charging end of the double-screw plastic extruding machine.
(II) preparation of a product:
(1) Porous polyvinyl chloride particles and nano TiO 2 Fully mixing cellulose nanocrystals and sodium lignin sulfonate by using a V-shaped particle mixer, and performing ball milling treatment to obtain a mixture 1; the ball milling treatment conditions are as follows: the rotating speed is 450r/min, and the ball-material ratio is 10:1, ball milling time is 15min.
(2) Fully mixing the mixture 1, the rubber wear-resistant agent, the calcium stearate, the polyol wax, the phosphate antioxidant and the calcined kaolin by using a V-shaped particle mixer, adding the mixture into a double-screw extruder, keeping the temperature of the front section in the double-screw extruder at 160-170 ℃, keeping the temperature of the middle section in the double-screw extruder at 160-165 ℃, keeping the temperature of the rear section at 140-150 ℃, and extruding the mixture to obtain the low-voc polyvinyl chloride plastic material.
The raw materials of the different examples are added in the following amounts (in parts by weight in the following table):
example 4
Unlike example 3, porous polyvinyl chloride particles B were used, the remainder being the same.
Example 5
Unlike example 3, porous polyvinyl chloride particles C were used, the remainder being the same.
Example 6
Unlike example 3, porous polyvinyl chloride particles D were used, the remainder being the same.
Comparative example 1
Unlike example 3, conventional polyvinyl chloride raw material particles (non-porous) were used instead of porous vinyl chloride particles, and the rest were the same.
Comparative example 2
Unlike example 3, sodium lignin sulfonate was not added, and the remainder were the same.
Comparative example 3
Unlike example 3, a mixture of 40% fully vulcanized powdered silicone rubber and 60% cellulose nanocrystals was used as the voc inhibitor instead of nano-TiO 2 The voc inhibitor, which is a combination of cellulose nanocrystals and sodium lignin sulfonate, is the same as the rest.
Comparative example 4
Unlike example 3, the ball milling treatment was not performed, and the rest was the same.
Result detection
The detection method comprises the following steps:
1. quantitative determination of total volatile organic compound content (TVOC): according to the German society of automotive industries standard VDA277.
2. Antibacterial properties: according to QB/T2591-2003, test method of antibacterial property and antibacterial effect of antibacterial plastics.
3. Tensile strength: the test standard was according to astm d 638.
4. Scratch resistance: standard according to the GWM14688 test.
Detection result:
| group of | TVOC(μg·C/g) | Antibacterial rate | Tensile Strength (MPa) | Scratch resistance DeltaL |
| Example 1 | 39 | 91.4 | 43.7 | 0.5 |
| Example 2 | 34 | 99.9 | 44.1 | 0.6 |
| Example 3 | 21 | 99.9 | 43.5 | 0.6 |
| Example 4 | 23 | 99.9 | 45.8 | 0.5 |
| Example 5 | 25 | 99.9 | 42.6 | 0.7 |
| Example 6 | 36 | 99.9 | 39.7 | 0.5 |
| Comparative example 1 | 67 | 99.9 | 45.2 | 0.7 |
| Comparative example 2 | 30 | 99.9 | 43.9 | 0.6 |
| Comparative example 3 | 46 | <70 | 40.3 | 0.5 |
| Comparative example 4 | 42 | 99.9 | 43.6 | 0.7 |
The result shows that the embodiment of the invention utilizes porous polyvinyl chloride to prepare the low-voc polyvinyl chloride plastic material, and the porous polyvinyl chloride and the nano TiO are adopted 2 Fiber and its preparation methodThe voc inhibitor compounded by the element nanocrystals and the sodium lignin sulfonate is fully adsorbed and contacted, and is further activated and mixed by ball milling, compared with the conventional nonporous polyvinyl chloride plastic material, the voc inhibitor has the advantages of obviously reducing the release amount of organic compounds, being safer and more environment-friendly, and simultaneously maintaining good physical properties. Comparative example 2 shows that sodium lignosulfonate is a key inhibitor composition for low-voc polyvinyl chloride plastic compounds prepared from porous polyvinyl chloride, and can significantly inhibit voc release after addition. In comparative example 3, a mixture of 40% fully vulcanized powdered silicone rubber and 60% cellulose nanocrystals was selected as the voc inhibitor, although having a certain inhibitory effect, the inhibitory effect against porous polyvinyl chloride was limited. Comparative example 4 shows that ball milling can increase inhibitor activity while allowing sufficient contact between the porous polyvinyl chloride and inhibitor, further reducing voc release.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (8)
1. The low-voc polyvinyl chloride plastic material is characterized by comprising the following components in parts by weight: 100 parts of porous polyvinyl chloride particles and nano TiO 2 1-15 parts of cellulose nanocrystals, 1-10 parts of sodium lignin sulfonate, 0.2-4 parts of rubber wear-resistant agent, 1-5 parts of calcium stearate, 0.05-0.5 part of polyol wax, 0.5-3 parts of phosphate antioxidant and 0-0.5 part of calcined kaolin, wherein the content of the phosphate antioxidant is not 0,
wherein the porosity of the porous polyvinyl chloride particles is 60-80%, and the pore diameter is 10-1000nm.
2. The low voc polyvinyl chloride plastic compound of claim 1, wherein the nano TiO 2 The D50 particle diameter of (2) is 5-50nm, and the D90 particle diameter is 10-100nm.
3. A low voc polyvinyl chloride plastic compound according to claim 1Characterized in that porous polyvinyl chloride particles and nano TiO 2 The mass ratio of cellulose nanocrystals to sodium lignin sulfonate is controlled at 20:2:1:0.1.
4. the low voc polyvinyl chloride plastic compound according to claim 3, wherein the low voc polyvinyl chloride plastic compound comprises the following components in parts by weight: 100 parts of porous polyvinyl chloride particles and nano TiO 2 10 parts of cellulose nanocrystals, 0.5 part of sodium lignin sulfonate, 2 parts of rubber wear-resistant agent, 0.1 part of calcium stearate, 1 part of polyol wax, 0.04 part of phosphate antioxidant and 15 parts of calcined kaolin.
5. A process for the preparation of a low voc polyvinyl chloride plastic compound according to any one of claims 1-4, comprising the steps of:
(1) Porous polyvinyl chloride particles and nano TiO 2 Fully mixing cellulose nanocrystals and sodium lignin sulfonate, and performing ball milling treatment to obtain a mixture 1;
(2) And (3) fully mixing the mixture 1, the rubber wear-resistant agent, calcium stearate, polyol wax, phosphate antioxidant and calcined kaolin, adding the mixture into a double-screw extruder, and extruding to obtain the low-voc polyvinyl chloride plastic material.
6. The method of preparing a low voc polyvinyl chloride plastic compound according to claim 5, wherein the mixing in steps (1) and (2) is performed by a V-shaped particle mixer.
7. The method for preparing a low voc polyvinyl chloride plastic compound according to claim 5, wherein in the step (1), the ball milling treatment conditions are as follows: the rotating speed is 100-1000r/min, and the ball-material ratio is 5-20:1, ball milling time is 5-20min.
8. The method for preparing a polyvinyl chloride plastic compound with low voc according to claim 5, wherein in the step (2), the temperature of the front stage in the twin-screw extruder is maintained at 160-170 ℃, the temperature of the middle stage is maintained at 160-165 ℃, and the temperature of the rear stage is maintained at 140-150 ℃.
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