CN112940426A - High-temperature water-soluble colored PVA (polyvinyl alcohol) particles and preparation method thereof - Google Patents
High-temperature water-soluble colored PVA (polyvinyl alcohol) particles and preparation method thereof Download PDFInfo
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- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
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- C08K3/20—Oxides; Hydroxides
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- C08K5/053—Polyhydroxylic alcohols
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- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
- C08K5/103—Esters; Ether-esters of monocarboxylic acids with polyalcohols
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- C08K5/00—Use of organic ingredients
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- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
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- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/37—Thiols
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- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
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Abstract
The invention relates to the field of biodegradable materials, in particular to high-temperature water-soluble colored PVA particles and a preparation method thereof. The high-temperature water-soluble colored PVA particle comprises the following components in parts by weight: 60-85 parts of PVA, 10-30 parts of polyol plasticizer, 0.1-1.5 parts of pigment, 0.05-0.1 part of surface treating agent, 0.5-6 parts of heat stabilizer, 0.5-8 parts of antioxidant, 1-5 parts of lubricant and 0.1-1 part of anti-hydrolysis agent. According to the invention, not only can continuous granulation of the high-temperature water-soluble PVA be realized, but also the problem of non-natural-color granulation of the PVA can be solved.
Description
Technical Field
The invention relates to the field of biodegradable materials, in particular to high-temperature water-soluble colored PVA particles and a preparation method thereof.
Background
In recent years, with the increasing demand of disposable non-degradable plastic products, environmental problems are highlighted, and the treatment and digestion of large quantities of non-degradable garbage become an urgent problem. Therefore, the biodegradable plastic enters the research field of people, and the biodegradable plastic can be completely degraded into carbon dioxide and water after the service life is finished, so that the harmless treatment to the environment is really realized.
Due to the excellent water solubility and degradability of polyvinyl alcohol, a great deal of research is done on biodegradable materials prepared by using polyvinyl alcohol at home and abroad. Particularly, the PVA material with alcoholysis degree of more than 99 percent can be used for producing and processing high-temperature (more than 80 ℃) water-soluble film materials, has wide use value, but has higher requirements on processing equipment and technology. In addition, the existing colored biodegradable film is obtained by blending biodegradable master batch and biodegradable master batch, and patents CN101475695, CN108059804 and the like disclose the master batch for PLA, PBAT and PCL biodegradable plastics, but no report on preparation of non-natural color PVA master batch or preparation of the master batch for PVA is available.
Disclosure of Invention
The invention aims to solve the problem that the fully alcoholysis PVA is easy to carbonize in the thermoplastic processing process in the prior art, realize continuous granulation of the PVA, provide a method for non-natural-color granulation of the PVA and overcome the problem that no color master batch for PVA film blowing is available at present.
In order to achieve the above object, a first aspect of the present invention provides a high temperature water-soluble colored PVA particle comprising: PVA, a polyol plasticizer, a pigment, a surface treatment agent, a heat stabilizer, an antioxidant, a lubricant and an anti-hydrolysis agent;
60-85 parts of PVA, 10-30 parts of polyol plasticizer, 0.1-1.5 parts of pigment, 0.01-0.05 part of surface treating agent, 0.5-6 parts of heat stabilizer, 0.5-8 parts of antioxidant, 1-5 parts of lubricant and 0.1-1 part of anti-hydrolysis agent.
Preferably, the polymerization degree of the PVA is 300-2600, the alcoholysis degree of the PVA is more than or equal to 99 percent, and the particle size of the PVA is 100-200 meshes.
Preferably, the polyol plasticizer is one or more of sorbitol, propylene glycol, glycerol, ethylene glycol 400, ethylene glycol 4000, ethylene glycol 20000, diglycerol, and diethylene glycol.
Preferably, the pigment includes an inorganic pigment and an organic pigment.
Preferably, the inorganic pigment is one or more of titanium dioxide, carbon black and iron oxide red; the organic pigment is one or more of phthalocyanine pigment, azo pigment and acridine pigment.
Preferably, the surface treatment agent is one or more of a titanate coupling agent, an aluminate coupling agent and a silane coupling agent.
Preferably, the heat stabilizer is one or more of an organic tin stabilizer, a rare earth stabilizer, a copper salt heat stabilizer, benzene diisooctyl phosphite, trialkyl phosphite, epoxy butyl stearate and epoxy soybean oil.
Preferably, the antioxidant is one or more of an antioxidant 697, an antioxidant 1024, an antioxidant 1076, an antioxidant 1098, an antioxidant 1010, an antioxidant 626, an antioxidant 168, an antioxidant DLTP and an antioxidant DSTP.
Preferably, the lubricant is one or more of liquid paraffin, polyethylene wax, oxidized polyethylene wax, erucamide, oleamide, triglycerol monostearate and pentaerythritol stearate.
Preferably, the anti-hydrolysis agent is one or more of N, N' -bis (2, 6-diisopropylphenyl) carbodiimide, poly-bis (1,3, 5-triisopropylphenyl) carbodiimide, and polymeric carbodiimide.
The invention provides a method for preparing high-temperature water-soluble colored PVA particles, which comprises the following steps:
a. weighing various raw materials according to the mass ratio of the components;
b. sequentially stirring the raw materials of the components at low speed and high speed in a high-speed mixer to obtain a mixed material;
c. and (3) extruding the mixed material in a single-screw extruder or a double-screw extruder, wherein the extrusion temperature is 45-220 ℃, the screw rotation speed is 200-450rpm, cooling and granulating to prepare the PVA particles.
The invention has the beneficial effects that:
the PVA plasticizing system after modification solves the problem of easy carbonization in the melting plasticizing process, and realizes the continuous granulation of the high-temperature water-soluble PVA.
The invention provides a preparation method of non-natural-color PVA master batch, which solves the problem that no master batch for PVA blown film exists at present.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The present invention will be described in detail below by way of examples. In the following examples, each material used was commercially available unless otherwise specified, and the method used was a conventional method in the art unless otherwise specified.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides high-temperature water-soluble colored PVA particles and a preparation method thereof, and the compatibility of pigment and auxiliary agent with PVA is improved by optimizing the components and the proportion of the high-temperature water-soluble colored PVA particles at the source of a granulation process, thereby realizing the feasibility of continuous granulation of PVA.
In a first aspect, the invention provides a high-temperature water-soluble colored PVA particle, which is prepared from the following raw materials in parts by weight:
60-85 parts of PVA, 10-30 parts of polyol plasticizer, 0.1-1.5 parts of pigment, 0.01-0.05 part of surface treating agent, 0.5-6 parts of heat stabilizer, 0.5-8 parts of antioxidant, 1-5 parts of lubricant and 0.1-1 part of anti-hydrolysis agent.
The PVA starting material is not particularly limited, but in the present invention, it is preferable that the PVA is a completely alcoholysis type PVA having a degree of alcoholysis of 99% and a degree of polymerization of 300-2600. In a specific example of the present invention, the PVA is selected from one or more of PVA0399, PVA0599, PVA1799, PVA2099, PVA2299, PVA2499 and PVA 2699.
The plasticizer is not particularly limited, and may be various plasticizers commonly used in the art, and may be determined by those skilled in the art according to the actual use requirement, and may be, for example, a small molecule polyol, a polyol ether, a fatty alcohol amine, or the like. In the present invention, preferably, the plasticizer is a polyol plasticizer, and the polyol plasticizer is one or more of sorbitol, propylene glycol, glycerin, ethylene glycol 400, ethylene glycol 4000, ethylene glycol 20000, diglycerin, and diethylene glycol.
In the present invention, preferably, the pigment includes an inorganic pigment and an organic pigment, and more preferably, the inorganic pigment is one or more of titanium dioxide, carbon black and iron oxide red; the organic pigment is one or more of phthalocyanine pigment, azo pigment and acridine pigment. The pigment functions to impart a beautiful appearance to the molded article.
The average particle size of the pigment is less than 400 meshes.
In the present invention, preferably, the surface treatment agent is one or more of a titanate coupling agent, an aluminate coupling agent, and a silane coupling agent. The interfacial bonding force between the inorganic powder material and the carrier resin is further improved by the surface treating agent.
The heat stabilizer is not particularly limited, and various heat stabilizers commonly used in the art may be used. In the present invention, preferably, the heat stabilizer is one or more of an organic tin stabilizer, a rare earth stabilizer, a copper salt heat stabilizer, benzene diisooctyl phosphite, trialkyl phosphite, epoxy butyl stearate and epoxy soybean oil. The heat stabilizer further ensures that the PVA is not decomposed and carbonized in the granulation process, inhibits the decomposition of the PVA and simultaneously provides a certain internal and external lubrication effect.
The antioxidant is not particularly limited, and may be various single-component antioxidants commonly used in the art. In the invention, preferably, the thermal-oxidative aging resistant agent is one or more of an antioxidant 697, an antioxidant 1024, an antioxidant 1076, an antioxidant 1098, an antioxidant 1010, an antioxidant 626, an antioxidant 168, an antioxidant DLTP and an antioxidant DSTP. The problem of decomposition and yellowing of PVA in processing is solved by introducing various antioxidants.
In the present invention, preferably, the lubricant is one or more of liquid paraffin, polyethylene wax, oxidized polyethylene wax, erucamide, oleamide, triglycerol monostearate, and pentaerythritol stearate. The processing performance of PVA during granulation is improved by the lubricant, and the melt flow rate of the particles is improved to a certain degree.
In the present invention, preferably, the anti-hydrolysis agent is one or more of N, N' -bis (2, 6-diisopropylphenyl) carbodiimide, poly-bis (1,3, 5-triisopropylphenyl) carbodiimide, and polymeric carbodiimide. By introducing the hydrolysis resistant agent, the water absorption of the PVA surface is prevented, and the water absorption of the PVA particles and the film is reduced.
In a second aspect, the present invention provides a method for preparing high temperature water soluble colored PVA particles, comprising the steps of:
a. weighing various raw materials according to the mass ratio of the components;
b. sequentially stirring the raw materials of the components at low speed and high speed in a high-speed mixer to obtain a mixed material;
c. extruding the mixed material in a single-screw extruder or a double-screw extruder at the extrusion temperature of 45-220 ℃ and the screw rotation speed of 200-450rpm, cooling and granulating to prepare PVA particles
The present invention will be described in detail below with reference to examples, but the present invention is not limited to the following examples.
All the starting materials used in the examples are commercially available, except where otherwise indicated.
Example 1
High temperature water soluble colored PVA particles comprising:
PVA179985 parts, glycerol 10 parts, phthalo cyanyl blue 1 part, aluminate coupling agent 0.01 part, titanate coupling agent 0.01 part, organic tin heat stabilizer 1 part, antioxidant 10101.48 part, pentaerythritol stearate 1 part, and N, N' -bis (2, 6-diisopropylphenyl) carbodiimide 0.5 part.
Example 2
High temperature water soluble colored PVA particles comprising:
5 parts of PVA209975 parts, 14 parts of ethylene glycol 40014 parts, 5 parts of glycerol, 1 part of titanium dioxide, 0.02 part of titanate coupling agent, 1 part of rare earth thermal stabilizer, 6971 parts of antioxidant, 10240.98 parts of antioxidant, 1 part of pentaerythritol stearate and 1 part of polymerized carbodiimide.
Example 3
High temperature water soluble colored PVA particles comprising:
PVA229980 parts, propylene glycol 5 parts, ethylene glycol 400010 parts, carbon black 0.8 part, titanate coupling agent 0.01 part, trialkyl phosphite 1 part, epoxy butyl stearate 0.89 part, antioxidant 10241 part, pentaerythritol stearate 1 part, and N, N' -bis (2, 6-diisopropylphenyl) carbodiimide 0.3 part.
Example 4
High temperature water soluble colored PVA particles comprising:
PVA249985 parts, sorbitol 10 parts, phthalo cyanyl blue 0.8 parts, titanate coupling agent 0.01 part, aluminate coupling agent 0.01 part, epoxidized soybean oil 0.5 part, epoxy butyl stearate 1 part, antioxidant DLTP 1.18 parts, liquid paraffin 1 part, and N, N' -bis (2, 6-diisopropylphenyl) carbodiimide 0.5 part.
Example 5
High temperature water soluble colored PVA particles comprising:
PVA059985 parts, ethylene glycol 40005 parts, sorbitol 5 parts, phthalocyanyl green 0.98 parts, titanate coupling agent 0.02 parts, rare earth stabilizer 0.5 parts, epoxidized soybean oil 0.5 parts, antioxidant 10980.5 parts, antioxidant DLTP 1 part, erucamide 1 part, and polymerized carbodiimide 0.5 part.
Example 6
High temperature water soluble colored PVA particles comprising:
PVA039980 parts, diethylene glycol 5 parts, propylene glycol 10 parts, titanium dioxide 0.98 parts, titanate coupling agent 0.02 parts, copper salt heat stabilizer 1 part, antioxidant 6971.7 parts, EVA wax 1 part, and polymerized carbodiimide 0.3 part.
Performance evaluation method:
the water content of the prepared high-temperature water-soluble colored PVA particles is tested according to the national standard GB/T6284-2006, and the melt flow rate is tested according to the national standard GB 3682-2000. The initial water-soluble temperature test method comprises the following steps: and (3) taking high-temperature water-soluble colored PVA particles which are quantitatively dried at 105 ℃ and have moisture removed, stirring the high-temperature water-soluble colored PVA particles at different water temperatures for 4 hours at a speed of 100r/min, drying and weighing the high-temperature water-soluble colored PVA particles, wherein the water temperature with the mass loss rate of more than 2 wt% is the initial water-soluble temperature of the PVA particles.
The above examples 1-6 were prepared according to the following procedure:
a. weighing various raw materials according to the mass ratio of the components;
b. sequentially stirring the raw materials of the components at a low speed and a high speed for 15 minutes in a high-speed mixer to obtain a mixed material;
c. extruding the mixed materials in a double-screw extruder, wherein the temperature of each area of the double screw is as follows: first zone 80 deg.C, second zone 100 deg.C, third zone 140 deg.C, fourth zone 160 deg.C, fifth zone 170 deg.C, sixth zone 180 deg.C, seventh zone 190 deg.C, eighth zone 190 deg.C, ninth zone 190 deg.C, tenth zone 195 deg.C, eleventh zone 200 deg.C, twelfth zone 205 deg.C, thirteenth zone 200 deg.C, and head 205 deg.C; setting the rotating speed of a screw to 300 rpm; then cooling and cutting into granules to prepare PVA particles S1-S6.
The high-temperature water-soluble colored PVA particles S1-S6 prepared as described above were subjected to the test, and the test results are shown in Table 1.
TABLE 1
As is clear from the results in Table 1, the high temperature water-soluble colored PVA grains prepared in examples S1 to S6 of the present invention have a relatively low water content (0.1 to 0.3%), are stable, do not affect thermoplastic processing, and do not generate blisters. The melt flow rates of examples S1-S6 were 2-5g/10min, and the flowability was appropriate to facilitate thermoplastic processing. Examples S1-S6 had initial water solubility temperatures of 90-95 ℃.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. High temperature water-soluble colored PVA particles, characterized in that they comprise: PVA, a polyol plasticizer, a pigment, a surface treatment agent, a heat stabilizer, an antioxidant, a lubricant and an anti-hydrolysis agent;
78-85 parts of PVA60, 10-30 parts of polyol plasticizer, 0.1-1.5 parts of pigment, 0.01-0.05 part of surface treating agent, 0.5-6 parts of heat stabilizer, 0.5-8 parts of antioxidant, 1-5 parts of lubricant and 0.1-1 part of anti-hydrolysis agent.
2. The high temperature water soluble colored PVA composition of claim 1, wherein the degree of polymerization of PVA is 300-2600;
preferably, the alcoholysis degree of the PVA is more than or equal to 99 percent;
preferably, the particle size of the PVA is 100-200 meshes.
3. The high temperature water soluble colored PVA particles of claim 1, wherein the polyol plasticizer is one or more of sorbitol, propylene glycol, glycerol, ethylene glycol 400, ethylene glycol 4000, ethylene glycol 20000, diglycerol, and diethylene glycol.
4. The high temperature water-soluble colored PVA particles according to claim 1, wherein the pigment comprises an organic pigment and an inorganic pigment, and has an average particle diameter of less than 400 mesh.
5. The high temperature water-soluble colored PVA particles according to claim 1, wherein the surface treatment agent is one or more of a titanate coupling agent, an aluminate coupling agent and a silane coupling agent.
6. The high temperature water soluble colored PVA particles of claim 1, wherein the heat stabilizer is one or more of an organotin stabilizer, a rare earth stabilizer, a copper salt heat stabilizer, diisooctyl phenyl phosphite, trialkyl phosphite, butyl epoxystearate, and epoxidized soybean oil.
7. The high temperature water soluble colored PVA particles of claim 1, wherein the antioxidant is one or more of antioxidant 697, antioxidant 1024, antioxidant 1076, antioxidant 1098, antioxidant 1010, antioxidant 626, antioxidant 168, antioxidant DLTP and antioxidant DSTP.
8. The high temperature water-soluble colored PVA particles of claim 1, wherein the lubricant is one or more of liquid paraffin, polyethylene wax, oxidized polyethylene wax, erucamide, oleamide, triglycerol monostearate and pentaerythritol stearate.
9. The high temperature water soluble colored PVA particles of claim 1, wherein the hydrolysis resistance agent is one or more of N, N' -bis (2, 6-diisopropylphenyl) carbodiimide, poly-bis (1,3, 5-triisopropylphenyl) carbodiimide, and polymeric carbodiimide.
10. A method for preparing high temperature water soluble colored PVA particles as claimed in any one of claims 1 to 9, comprising the steps of:
a. weighing various raw materials according to the mass ratio of the components;
b. sequentially stirring the raw materials of the components at low speed and high speed in a high-speed mixer to obtain a mixed material;
c. and (3) extruding the mixed material in a single-screw extruder or a double-screw extruder, wherein the extrusion temperature is 45-220 ℃, the screw rotation speed is 200-450rpm, cooling and granulating to prepare the PVA particles.
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