CN111995834A - Modified particle based on PVA/starch and preparation method thereof - Google Patents
Modified particle based on PVA/starch and preparation method thereof Download PDFInfo
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- CN111995834A CN111995834A CN202010845696.3A CN202010845696A CN111995834A CN 111995834 A CN111995834 A CN 111995834A CN 202010845696 A CN202010845696 A CN 202010845696A CN 111995834 A CN111995834 A CN 111995834A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L29/00—Compositions 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 an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
- C08L29/02—Homopolymers or copolymers of unsaturated alcohols
- C08L29/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention relates to a method for preparing modified particles based on PVA/starch by using a double-screw extruder, which is prepared from the following raw materials in parts by weight: 50-90 parts by weight of high-temperature water-soluble PVA resin; 10-50 parts of starch; 10-40 parts by weight of a plasticizer; 1-6 parts of a thermal stabilizer; 1-6 parts by weight of a lubricant; 0.5-2 parts of antioxidant. The PVA/starch modified particles are prepared by blending, drying and preplasticizing the materials through a blender and granulating through a 35 granulator. The beneficial effects of the invention are: (1) the processing window of PVA melting granulation is widened, and the problems that PVA is easy to decompose and turn yellow during granulation and the like are solved. (2) The addition of the starch reduces the production and processing cost. (3) The thermal stabilizer improves the thermal stability of PVA and starch. (4) The PVA/starch modified particles after being granulated by the double screw can be directly used for melting and film blowing, and has the characteristics of low investment, high productivity, low energy consumption and the like.
Description
Technical Field
The invention belongs to the technical field of biodegradable materials, and particularly relates to modified particles based on PVA/starch and a preparation method thereof.
Background
In recent years, the demand for plastic packaging products is increasing, and to a certain extent, the plastic packaging is used as an integral part of the packaging of food, fruits and vegetables, daily chemicals and the like, and the plastic packaging is more widely applied to daily life and food storage. Therefore, the requirement of people on environmental protection is increased day by day, and the plastic packaging product is required to have higher performance and multiple functions, and is further required to have no pollution and public nuisance to food, people and environment. Therefore, research has been focused on moving to new plastic packaging materials that do not degrade in a contaminating manner.
The PVA film is soluble in water, has high mechanical property, good transparency and high oil resistance and corrosion resistance, enters the visual field of people at the initial stage of the 20 th century, and is rapidly developed at home and abroad. In the production process of PVA film, the melting temperature is close to the decomposition temperature, so the melt extrusion method has high processing difficulty in industrial production, and the casting method is mostly used for film forming. In the modification production of PVA films, Japan is to develop a high temperature (80 ℃) resistant water-soluble PVA film in advance of other countries, and creates favorable conditions for the wide application of the PVA film. Although the research on the water and temperature resistance of the PVA film in China is advanced to a certain extent, the intermediate temperature PVA film which has the advantages of low water and temperature resistance (60 ℃), easy curling in water and easy moisture absorption at normal temperature and wrinkling is developed, and the defects cause that downstream products cannot be continuously researched and developed, so that the popularization and the use of the PVA film are limited. The development of domestic high-temperature polyvinyl alcohol films is not broken through, the sources only depend on import, and the use cost is greatly improved.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides modified particles based on PVA/starch and a preparation method thereof. According to the invention, PVA is modified at the source of the granulation process, so that the prepared PVA/starch modified particles are heated stably, the feasibility of high-temperature water-soluble PVA granulation is realized, and the production cost is reduced while the environment is protected.
In order to achieve the above object, a first aspect of the present invention provides a PVA/starch-based modified particle comprising the following components in parts by weight:
50-90 parts of high-temperature water-soluble PVA resin, 10-50 parts of starch, 10-40 parts of plasticizer, 1-6 parts of heat stabilizer, 1-6 parts of lubricant and 0.5-3 parts of antioxidant.
Preferably, the high temperature water-soluble PVA resin is selected from one or more of designations 0899, 1099, 1599, 1799, 2099, 2299, 2499 and 2699.
Preferably, the starch is one or more selected from corn starch, potato starch, tapioca starch, wheat starch and acetate starch.
Preferably, the plasticizer is selected from one or more of propylene glycol, glycerol, sorbitol, polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 800, mannitol, trimethylolpropane, tetrahydroxymethyl propane, span 20, span 60, span 80, tween 20, tween 40 and tween 60.
Preferably, the thermal stabilizer is selected from one or more of glyceryl monostearate, glyceryl tristearate, glyceryl triglycerol monostearate, laurate and sorbitan stearate.
Preferably, the lubricant is selected from one or more of zinc stearate, calcium stearate, magnesium stearate, barium stearate, stearic acid, stearyl alcohol, stearamide, erucamide, oleamide, hydroxystearic acid and myristic acid.
Preferably, the antioxidant is selected from one or more of antioxidant 1010, antioxidant 1076, antioxidant 1098, antioxidant 1024, antioxidant 697, antioxidant 565, antioxidant DSTDP, antioxidant DLTDP, antioxidant 618, antioxidant 168 and antioxidant 626.
In a second aspect, the present invention provides a method for preparing modified particles based on PVA/starch, the method comprising: putting starch, plasticizer and thermal stabilizer into a high-speed mixer, mixing for 5-15 minutes at 30-70 ℃ to pre-plasticize the starch, then adding high-temperature water-soluble PVA resin and other auxiliaries into the high-speed mixer, mixing for 10-20 minutes at 50-90 ℃, drying for 4-8 hours at 70-100 ℃, and granulating to obtain the starch-based heat stabilizer.
Preferably, the granulator used for granulation is a granulator with a screw length-diameter ratio of 44-52: 1 twin-screw granulator.
The PVA is modified at the source of the granulation process, so that the PVA/starch modified particles which are stable to heat are prepared. The feasibility of granulating the high-temperature water-soluble PVA is realized, and the cost is greatly reduced by adding the starch while the environmental protection is realized.
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.
In a first aspect, the present invention provides a PVA/starch-based modified particle, a PVA/starch modified particle, comprising in parts by weight:
50-90 parts of high-temperature water-soluble PVA resin, 10-50 parts of starch, 10-40 parts of plasticizer, 1-6 parts of heat stabilizer, 1-6 parts of lubricant and 0.5-3 parts of antioxidant.
In the present invention, preferably, the particles comprise the following components in parts by weight:
60-80 parts of high-temperature water-soluble PVA resin, 20-50 parts of starch, 10-40 parts of plasticizer, 2-6 parts of heat stabilizer, 2-6 parts of lubricant and 1-2.5 parts of antioxidant.
In the present invention, preferably, the high temperature water-soluble PVA resin is selected from one or more of the group consisting of trade names 0899, 1099, 1599, 1799, 2099, 2299, 2499 and 2699.
In the present invention, preferably, one or more of corn starch, potato starch, tapioca starch, wheat starch and acetate starch.
The mesh number of the starch can be 300-800 meshes.
In the present invention, preferably, the plasticizer is selected from one or more of propylene glycol, glycerol, sorbitol, polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 800, mannitol, trimethylolpropane, tetramethylolpropane, span 20, span 60, span 80, tween 20, tween 40 and tween 60, and more preferably, a compound plasticizer of two or more.
The compound plasticizer is preferably the combination of propylene glycol and/or glycerol and one or more of polyethylene glycol, tetrahydroxymethyl propane and sorbitol. In a specific embodiment of the present invention, a combination of propylene glycol and glycerol and any one of polyethylene glycol, tetramethylolpropane and sorbitol is selected.
In the present invention, preferably, the heat stabilizer is selected from one or more, more preferably two or more, of glyceryl monostearate, glyceryl tristearate, glyceryl triglycerol monostearate, laurate and sorbitan stearate.
In the present invention, preferably, the lubricant is one or more selected from zinc stearate, calcium stearate, magnesium stearate, barium stearate, stearic acid, stearyl alcohol, stearamide, erucamide, oleamide, hydroxystearic acid and myristic acid, and more preferably, two or more are used in combination.
The compound lubricant is preferably a combination of calcium stearate and magnesium stearate, and more preferably the weight ratio of the calcium stearate to the magnesium stearate is 1: 1; the above compounded lubricant may also preferably be a combination of hydroxystearic acid and erucamide, more preferably in a weight ratio of 1: 1.
In the present invention, preferably, the antioxidant is selected from one or more of antioxidant 1010, antioxidant 1076, antioxidant 1098, antioxidant 1024, antioxidant 697, antioxidant 565, antioxidant DSTDP, antioxidant DLTDP, antioxidant 618, antioxidant 168 and antioxidant 626, and more preferably, the primary and secondary antioxidants are used in a synergistic manner.
In a second aspect, the present invention provides a method for preparing modified particles based on PVA/starch, the method comprising: putting starch, plasticizer and thermal stabilizer into a high-speed mixer, mixing for 5-15 minutes at 30-80 ℃ to pre-plasticize the starch, then adding high-temperature water-soluble PVA resin and other auxiliaries into the high-speed mixer, mixing for 10-20 minutes at 50-90 ℃, drying for 4-8 hours at 70-100 ℃, and granulating to obtain the starch-based heat stabilizer.
Specifically, the preparation method comprises the following steps: respectively plasticizing starch and PVA with a compound plasticizer in a high-speed mixer at 40-75 ℃ for 5-10 minutes, then mixing the starch and PVA with other auxiliary agents together for 5-8 minutes, placing the mixed powder into an air-blast drying oven at 70-95 ℃ for heating for 5-7 hours to ensure that the moisture content in the material is 0.5-3 wt%, and then discharging the material at room temperature for later use.
Further preferably, the granulation in the preparation method is as follows: adding the mixed and dried powder into a screw with the length-diameter ratio of 44-52: 1 a double-screw 35 granulator with forced feeding, wherein the main feeding speed is 15-38r/min, the main machine rotating speed is 300-450r/min, the temperature is 150-210 ℃, and finally the PVA/starch modified particles are obtained through melt extrusion, air cooling and drawing and granulation.
As PVA and starch both belong to hydrophilic materials, are easy to absorb moisture and have higher water content, in the prior art, when PVA/starch particles are prepared, even if the vacuum is opened to the maximum, pores or blisters also appear in the particles, and a plurality of defects are generated during film forming. The invention dries the mixed powder, which is more beneficial to the plasticization of PVA and starch during drying.
Since PVA and starch both belong to polyhydroxy high molecular polymers, a large number of hydrogen bonds are contained in molecules and among molecules, and the PVA and the starch begin to decompose when molten or not. The invention introduces the compound plasticizer, solves the problem of poor plasticizing effect of a single plasticizer, destroys hydrogen bonds in molecules and among molecules of PVA and starch, ensures that the micromolecule plasticizer can easily enter the interior of the molecules for plasticizing, and widens the processing window of PVA.
The invention introduces a plurality of heat stabilizers, and solves the problem that PVA and starch are decomposed and turn yellow in the processing process.
The invention adopts a brand new mixing system of separately plasticizing, then blending and drying, has better plasticizing effect and greatly reduces the water content, and solves the problem that the particles still have air holes and water bubbles after vacuumizing.
The method has the beneficial effects of widening the processing window of PVA melting granulation and solving the problems of easy decomposition and yellowing of PVA during granulation and the like. The addition of the starch reduces the production and processing cost. The thermal stabilizer improves the thermal stability of PVA and starch. The modified PVA resin after being granulated by the double screw can be directly used for melting and film blowing, and has the characteristics of low investment, high productivity, low energy consumption and the like.
In order to illustrate the present invention in more detail, the modified PVA/starch particles and the method for producing the same according to the present invention will be specifically described below with reference to examples.
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
179990 parts by weight of polyvinyl alcohol, 10 parts by weight of corn starch, 5 parts by weight of propylene glycol, 5 parts by weight of glycerol, 2005 parts by weight of polyethylene glycol, 3 parts by weight of glyceryl monostearate, 1 part by weight of calcium stearate, 1 part by weight of magnesium stearate, 10100.8 parts by weight of antioxidant and 0.5 part by weight of antioxidant DSTDP.
Example 2
179990 parts by weight of polyvinyl alcohol, 10 parts by weight of corn starch, 5 parts by weight of propylene glycol, 8 parts by weight of glycerol, 2005 parts by weight of polyethylene glycol, 3 parts by weight of glyceryl monostearate, 1 part by weight of calcium stearate, 1 part by weight of magnesium stearate, 10100.8 parts by weight of antioxidant and 0.5 part by weight of antioxidant DSTDP.
Example 3
249990 parts of polyvinyl alcohol, 10 parts of corn starch, 5 parts of propylene glycol, 5 parts of glycerol, 2008 parts of polyethylene glycol, 3 parts of glyceryl monostearate, 1 part of calcium stearate, 1 part of magnesium stearate, 10100.8 parts of antioxidant and 0.5 part of antioxidant DSTDP.
Example 4
249990 parts of polyvinyl alcohol, 10 parts of corn starch, 5 parts of propylene glycol, 5 parts of glycerol, 5 parts of tetramethylolpropane, 3 parts of glyceryl monostearate, 1 part of calcium stearate, 1 part of magnesium stearate, 10100.8 parts of antioxidant and 0.5 part of antioxidant DSTDP.
Example 5
179990 parts by weight of polyvinyl alcohol, 10 parts by weight of corn starch, 5 parts by weight of propylene glycol, 5 parts by weight of glycerol, 8 parts by weight of tetramethylolpropane, 3 parts by weight of glyceryl monostearate, 1 part by weight of calcium stearate, 1 part by weight of magnesium stearate, 10100.8 parts by weight of antioxidant and 0.5 part by weight of antioxidant DSTDP.
Example 6
179990 parts by weight of polyvinyl alcohol, 10 parts by weight of corn starch, 5 parts by weight of propylene glycol, 5 parts by weight of glycerol, 5 parts by weight of tetramethylolpropane, 3 parts by weight of glyceryl monostearate, 1 part by weight of hydroxystearic acid, 1 part by weight of erucamide, 10100.8 parts by weight of antioxidant and 0.5 part by weight of antioxidant DSTDP.
Example 7
089990 parts of polyvinyl alcohol, 10 parts of corn starch, 5 parts of propylene glycol, 5 parts of glycerol, 5 parts of trimethylolpropane, 3 parts of glyceryl monostearate, 1 part of hydroxystearic acid, 1 part of erucamide, 10100.8 parts of antioxidant and 0.5 part of antioxidant DSTDP.
Example 8
089910 parts of polyvinyl alcohol, 179970 parts of PVA, 20 parts of acetate starch, 5 parts of propylene glycol, 5 parts of glycerol, 8 parts of trimethylolpropane, 3 parts of glycerin monostearate, 1 part of hydroxystearic acid, 1 part of erucamide, 10100.8 parts of antioxidant and 0.5 part of antioxidant DSTDP.
Example 9
179980 parts of polyvinyl alcohol, 20 parts of acetate starch, 5 parts of propylene glycol, 5 parts of glycerol, 8 parts of tetramethylolpropane, 3 parts of glyceryl monostearate, 1 part of hydroxystearic acid, 1 part of erucamide, 10100.8 parts of antioxidant and 0.5 part of antioxidant DSTDP.
Example 10
179980 parts of polyvinyl alcohol, 20 parts of acetate starch, 5 parts of propylene glycol, 8 parts of glycerol, 5 parts of sorbitol, 3 parts of glyceryl monostearate, 1 part of hydroxystearic acid, 1 part of erucamide, 10100.8 parts of antioxidant and 0.5 part of antioxidant DSTDP.
Preparation of PVA/starch modified particles
According to the specific implementation mode, firstly, according to the proportion shown in examples 1-10, starch and PVA are respectively plasticized with compound plasticizer in a high-speed mixer for 10 minutes at 70 ℃, then are mixed with other auxiliary agents together and dispersed for 8 minutes, the mixed powder is put into a blowing drying oven at 90 ℃ to be heated for 6 hours, so that the moisture content in the material is lower than 1 wt%, and then the material is discharged to room temperature for standby. Then adding the mixed and dried powder into a screw with the length-diameter ratio of 44: 1 in a double-screw 35 granulator with forced feeding, the main feeding speed is 28r/min, the main machine rotating speed is 380r/min, and the temperature of each area of the double-screw extruder is set as follows: the PVA/starch modified particles are obtained by melting extrusion, air-cooling stretching and granulation at 90 ℃ in the first area, 140 ℃ in the second area, 150 ℃ in the third area, 150 ℃ in the fourth area, 160 ℃ in the fifth area, 160 ℃ in the sixth area, 170 ℃ in the seventh area, 175 ℃ in the eighth area, 175 ℃ in the ninth area, 180 ℃ in the tenth area, 185 ℃ in the eleventh area, 190 ℃ in the twelfth area, 200 ℃ in the tenth area and 200 ℃ in a nose.
Performance evaluation method:
and (3) testing the water content of the prepared modified particles according to the national standard GB/T6284-2006, testing the melt index of the modified particles according to the national standard GB3682-2000, injection-molding the PVA/starch modified particles into injection-molded sample strips according to the national standard GB/T1040 by using an injection molding machine with the model number TY-7003, and testing the tensile strength and the elongation at break of the sample strips.
The results of the performance tests of examples 1-10 of PVA/starch modified particles of the invention are shown in Table 1 below.
TABLE 1
The above description is only of the preferred embodiments of the present invention, but the scope of the present invention is not limited thereto. Within the scope of the design concept of the present invention, many simple modifications may be made to the technical solution of the present invention, including combinations of various technical features in any other suitable manner, and these simple modifications and combinations should also be regarded as the disclosure of the present invention, and all fall within the scope of the present invention.
Claims (9)
1. Modified particles based on PVA/starch, characterized in that the particles comprise the following components in parts by weight:
50-90 parts of high-temperature water-soluble PVA resin, 10-50 parts of starch, 10-40 parts of plasticizer, 1-6 parts of heat stabilizer, 1-6 parts of lubricant and 0.5-3 parts of antioxidant.
2. The PVA/starch-based modified particle as claimed in claim 1, wherein the high temperature water-soluble PVA resin is selected from one or more of trade names 0899, 1099, 1599, 1799, 2099, 2299, 2499 and 2699.
3. The PVA/starch-based modified particle of claim 1, wherein said starch is one or more selected from the group consisting of corn starch, potato starch, tapioca starch, wheat starch and acetate starch.
4. The PVA/starch-based modified particle of claim 1, wherein said plasticizer is selected from one or more of propylene glycol, glycerol, sorbitol, polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 800, mannitol, trimethylolpropane, tetramethylolpropane, span 20, span 60, span 80, Tween 20, Tween 40 and Tween 60.
5. The PVA/starch-based modified particle of claim 1, wherein said thermal stabilizer is selected from one or more of glyceryl monostearate, glyceryl tristearate, glyceryl triglycerol monostearate, laurate and sorbitan stearate.
6. The PVA/starch-based modified particle of claim 1, wherein said lubricant is selected from one or more of zinc stearate, calcium stearate, magnesium stearate, barium stearate, stearic acid, stearyl alcohol, stearamide, erucamide, oleamide, hydroxystearic acid and myristic acid.
7. The PVA/starch-based modified particle of claim 1, wherein said antioxidant is selected from one or more of antioxidant 1010, antioxidant 1076, antioxidant 1098, antioxidant 1024, antioxidant 697, antioxidant 565, antioxidant DSTDP, antioxidant DLTDP, antioxidant 618, antioxidant 168 and antioxidant 626.
8. A preparation method of modified particles based on PVA/starch is characterized by comprising the following steps: putting starch, plasticizer and thermal stabilizer into a high-speed mixer, mixing for 5-15 minutes at 30-80 ℃ to pre-plasticize the starch, then adding high-temperature water-soluble PVA resin and other auxiliaries into the high-speed mixer, mixing for 10-20 minutes at 50-90 ℃, drying for 4-8 hours at 70-100 ℃, and granulating to obtain the starch-based heat stabilizer.
9. The PVA/starch-based modified particle of claim 8, wherein the granulation is carried out using a granulator having a screw length to diameter ratio of 44 to 52: 1 twin-screw granulator.
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| CN202010845696.3A CN111995834A (en) | 2020-08-20 | 2020-08-20 | Modified particle based on PVA/starch and preparation method thereof |
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| CN202010845696.3A CN111995834A (en) | 2020-08-20 | 2020-08-20 | Modified particle based on PVA/starch and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115322504A (en) * | 2022-08-24 | 2022-11-11 | 山东鲁仁高分子材料有限公司 | PVA (polyvinyl alcohol) foaming resin suitable for simple foaming equipment and preparation method thereof |
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2020
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115322504A (en) * | 2022-08-24 | 2022-11-11 | 山东鲁仁高分子材料有限公司 | PVA (polyvinyl alcohol) foaming resin suitable for simple foaming equipment and preparation method thereof |
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Application publication date: 20201127 |