WO2023103116A1 - Special biomass color masterbatch for degradable plastic and preparation method therefor - Google Patents
Special biomass color masterbatch for degradable plastic and preparation method therefor Download PDFInfo
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- WO2023103116A1 WO2023103116A1 PCT/CN2021/141983 CN2021141983W WO2023103116A1 WO 2023103116 A1 WO2023103116 A1 WO 2023103116A1 CN 2021141983 W CN2021141983 W CN 2021141983W WO 2023103116 A1 WO2023103116 A1 WO 2023103116A1
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- color masterbatch
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- 239000004595 color masterbatch Substances 0.000 title claims abstract description 49
- 229920006238 degradable plastic Polymers 0.000 title claims abstract description 49
- 239000002028 Biomass Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229920000747 poly(lactic acid) Polymers 0.000 claims abstract description 67
- 239000004626 polylactic acid Substances 0.000 claims abstract description 67
- 239000003063 flame retardant Substances 0.000 claims abstract description 29
- 239000011256 inorganic filler Substances 0.000 claims abstract description 25
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 25
- 239000004014 plasticizer Substances 0.000 claims abstract description 25
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 23
- 239000006097 ultraviolet radiation absorber Substances 0.000 claims abstract description 22
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims abstract description 21
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims abstract description 17
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 239000003086 colorant Substances 0.000 claims abstract description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 36
- 238000002156 mixing Methods 0.000 claims description 32
- 238000003756 stirring Methods 0.000 claims description 32
- 239000000975 dye Substances 0.000 claims description 29
- 239000000463 material Substances 0.000 claims description 25
- 241000196324 Embryophyta Species 0.000 claims description 24
- 229920000805 Polyaspartic acid Polymers 0.000 claims description 24
- 239000012456 homogeneous solution Substances 0.000 claims description 24
- 108010064470 polyaspartate Proteins 0.000 claims description 24
- 239000002994 raw material Substances 0.000 claims description 17
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 16
- 239000000839 emulsion Substances 0.000 claims description 16
- 238000001125 extrusion Methods 0.000 claims description 16
- 235000011187 glycerol Nutrition 0.000 claims description 16
- ZQBAKBUEJOMQEX-UHFFFAOYSA-N salicylic acid phenyl ester Natural products OC1=CC=CC=C1C(=O)OC1=CC=CC=C1 ZQBAKBUEJOMQEX-UHFFFAOYSA-N 0.000 claims description 16
- 239000008096 xylene Substances 0.000 claims description 16
- 239000003963 antioxidant agent Substances 0.000 claims description 14
- 230000003078 antioxidant effect Effects 0.000 claims description 11
- 229920005989 resin Polymers 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 10
- 241001070941 Castanea Species 0.000 claims description 8
- 235000014036 Castanea Nutrition 0.000 claims description 8
- 239000005909 Kieselgur Substances 0.000 claims description 8
- 240000002853 Nelumbo nucifera Species 0.000 claims description 8
- 235000006508 Nelumbo nucifera Nutrition 0.000 claims description 8
- 235000006510 Nelumbo pentapetala Nutrition 0.000 claims description 8
- 241000510091 Quadrula quadrula Species 0.000 claims description 8
- 235000014220 Rhus chinensis Nutrition 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 244000046101 Sophora japonica Species 0.000 claims description 8
- 235000010586 Sophora japonica Nutrition 0.000 claims description 8
- 235000005865 Symphytum officinale Nutrition 0.000 claims description 8
- 230000008014 freezing Effects 0.000 claims description 8
- 238000007710 freezing Methods 0.000 claims description 8
- 238000005469 granulation Methods 0.000 claims description 8
- 230000003179 granulation Effects 0.000 claims description 8
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical group [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 8
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 8
- 239000000347 magnesium hydroxide Substances 0.000 claims description 8
- 239000004005 microsphere Substances 0.000 claims description 8
- 238000005191 phase separation Methods 0.000 claims description 8
- 239000001575 punica granatum l. bark extract Substances 0.000 claims description 8
- 229940119485 safflower extract Drugs 0.000 claims description 8
- 235000012424 soybean oil Nutrition 0.000 claims description 8
- 239000003549 soybean oil Substances 0.000 claims description 8
- 235000003332 Ilex aquifolium Nutrition 0.000 claims description 7
- 235000002296 Ilex sandwicensis Nutrition 0.000 claims description 7
- 235000002294 Ilex volkensiana Nutrition 0.000 claims description 7
- 229940069521 aloe extract Drugs 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 235000000857 Pentadesma butyracea Nutrition 0.000 claims 1
- 240000003152 Rhus chinensis Species 0.000 claims 1
- 244000057114 Sapium sebiferum Species 0.000 claims 1
- 240000002299 Symphytum officinale Species 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 3
- 230000004048 modification Effects 0.000 abstract description 3
- 229940124543 ultraviolet light absorber Drugs 0.000 abstract 1
- 241000208225 Rhus Species 0.000 description 7
- 241001442052 Symphytum Species 0.000 description 7
- 229920003023 plastic Polymers 0.000 description 7
- 239000004033 plastic Substances 0.000 description 7
- 239000003760 tallow Substances 0.000 description 7
- 235000013311 vegetables Nutrition 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000006096 absorbing agent Substances 0.000 description 3
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- 238000006065 biodegradation reaction Methods 0.000 description 2
- 229940097362 cyclodextrins Drugs 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229920000856 Amylose Polymers 0.000 description 1
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 102000000340 Glucosyltransferases Human genes 0.000 description 1
- 108010055629 Glucosyltransferases Proteins 0.000 description 1
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- 229920000881 Modified starch Polymers 0.000 description 1
- 239000004368 Modified starch Substances 0.000 description 1
- 241000209504 Poaceae Species 0.000 description 1
- 235000014104 aloe vera supplement Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000009264 composting Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- -1 cyclic oligosaccharides Chemical class 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000001398 gaultheria procumbens l. leaf extract Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 235000019426 modified starch Nutrition 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 1
- 229920001542 oligosaccharide Polymers 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
-
- 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
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/16—Cyclodextrin; Derivatives thereof
-
- 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
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0041—Optical brightening agents, organic pigments
Definitions
- the invention provides a special biomass color masterbatch for degradable plastics.
- step (2) Add polyaspartic acid solution to the homogeneous solution obtained in step (1), adjust the temperature value to 50°C, and keep stirring for 40min to obtain an intermediate solution;
- the mass fraction of the polyaspartic acid solution is 10%
- the inorganic filler is diatomaceous earth.
- Figure 1 is a graph showing the influence of the added weight of modified starch on the tensile strength.
- step (3) Add glycerin to the intermediate solution obtained in step (2), stir with 3000r/min rotating speed for 40min, obtain emulsion;
- the mass fraction of the polyaspartic acid solution is 10%
- the plant dyeing agent is Sophora japonica extract, sumac extract, comfrey extract, holly leaf extract, safflower extract, acorn extract, tallow leaf extract, pomegranate peel extract, lotus leaf extract , maple leaf extract, aloe extract, chestnut shell extract in one or more.
- the flame retardant is magnesium hydroxide.
- Described plasticizer is epoxidized soybean oil.
- the anti-aging agent is: N-phenyl- ⁇ -aniline;
- a special biomass color masterbatch for degradable plastics made of the following components in parts by weight: 23 parts of vegetable dyes, 24 parts of cyclodextrin, 2 parts of flame retardants, 37 parts of modified polylactic acid, and 1.8 parts of plasticizers parts, 1.6 parts of ultraviolet absorbers, 1.4 parts of antioxidants, 6.8 parts of inorganic fillers, and 0.35 parts of sodium stearate.
- the preparation method of the modified polylactic acid resin is:
- step (3) Add glycerin to the intermediate solution obtained in step (2), stir with 3000r/min rotating speed for 40min, obtain emulsion;
- the mixing mass ratio of polylactic acid and xylene is 1:12.
- the mass fraction of the polyaspartic acid solution is 10%
- the plant dyeing agent is Sophora japonica extract, sumac extract, comfrey extract, holly leaf extract, safflower extract, acorn extract, tallow leaf extract, pomegranate peel extract, lotus leaf extract , maple leaf extract, aloe extract, chestnut shell extract in one or more.
- the flame retardant is magnesium hydroxide.
- Described plasticizer is epoxidized soybean oil.
- the ultraviolet absorber is phenyl o-hydroxybenzoate.
- a preparation method of special biomass color masterbatch for degradable plastics comprising the following steps:
- Described plasticizer is epoxidized soybean oil.
- step (2) Add polyaspartic acid solution to the homogeneous solution obtained in step (1), adjust the temperature value to 50° C., and keep stirring for 40 minutes to obtain an intermediate solution;
- step (3) Add glycerin to the intermediate solution obtained in step (2), stir with 3000r/min rotating speed for 40min, obtain emulsion;
- the mixing mass ratio of polylactic acid and xylene is 1:12.
- the mixing mass ratio of the homogeneous solution and the polyaspartic acid solution is 5:1;
- the ultraviolet absorber is phenyl o-hydroxybenzoate.
- the anti-aging agent is: N-phenyl- ⁇ -aniline;
- the extrusion temperature of the twin-screw extruder is 200°C.
- step (2) Add polyaspartic acid solution to the homogeneous solution obtained in step (1), adjust the temperature value to 50° C., and keep stirring for 40 minutes to obtain an intermediate solution;
- the mixing mass ratio of polylactic acid and xylene is 1:12.
- the mass fraction of the polyaspartic acid solution is 10%
- the mixing mass ratio of the intermediate solution and glycerin is 5:2.
- the plant dyeing agent is Sophora japonica extract, sumac extract, comfrey extract, holly leaf extract, safflower extract, acorn extract, tallow leaf extract, pomegranate peel extract, lotus leaf extract , maple leaf extract, aloe extract, chestnut shell extract in one or more.
- the flame retardant is magnesium hydroxide.
- Described plasticizer is epoxidized soybean oil.
- the ultraviolet absorber is phenyl o-hydroxybenzoate.
- the anti-aging agent is: N-phenyl- ⁇ -aniline;
- the inorganic filler is diatomaceous earth.
- a preparation method of special biomass color masterbatch for degradable plastics comprising the following steps:
- the extrusion temperature of the twin-screw extruder is 200°C.
- a special biomass color masterbatch for degradable plastics made of the following components in parts by weight: 26 parts of vegetable dyes, 25 parts of cyclodextrin, 3 parts of flame retardants, 40 parts of modified polylactic acid, and 3 parts of plasticizers 2 parts, 2 parts of ultraviolet absorber, 1.6 parts of antioxidant, 7 parts of inorganic filler, 0.5 part of sodium stearate.
- the preparation method of the modified polylactic acid resin is:
- step (2) Add polyaspartic acid solution to the homogeneous solution obtained in step (1), adjust the temperature value to 50° C., and keep stirring for 40 minutes to obtain an intermediate solution;
- step (3) Add glycerin to the intermediate solution obtained in step (2), stir with 3000r/min rotating speed for 40min, obtain emulsion;
- step (3) The emulsion obtained in step (3) is subjected to freezing phase separation, and after the polylactic acid is solidified into microspheres, it is washed and separated to obtain modified polylactic acid.
- the mixing mass ratio of polylactic acid and xylene is 1:12.
- the mixing mass ratio of the homogeneous solution and the polyaspartic acid solution is 5:1;
- the mixing mass ratio of the intermediate solution and glycerin is 5:2.
- the plant dyeing agent is Sophora japonica extract, sumac extract, comfrey extract, holly leaf extract, safflower extract, acorn extract, tallow leaf extract, pomegranate peel extract, lotus leaf extract , maple leaf extract, aloe extract, chestnut shell extract in one or more.
- the flame retardant is magnesium hydroxide.
- Described plasticizer is epoxidized soybean oil.
- the ultraviolet absorber is phenyl o-hydroxybenzoate.
- the inorganic filler is diatomaceous earth.
- a preparation method of special biomass color masterbatch for degradable plastics comprising the following steps:
- the extrusion temperature of the twin-screw extruder is 200°C.
- Comparative Example 1 The difference from Example 1 is that the modified polylactic acid resin is replaced by the unmodified polylactic acid;
- Comparative Example 1 The difference from Example 1 is that the modified polylactic acid resin is replaced by the unmodified polylactic acid;
- Blank control group application number 201310360960.4, a degradable plastic and a plastic prepared by its preparation method;
- Example 1 As the basic sample, application number 201310360960.4, a degradable plastic and a plastic prepared by its preparation method, as the test sample, compare the effects of different addition ratios of Examples on the tensile strength of the degradable plastic.
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
A special biomass color masterbatch for a degradable plastic and a preparation method therefor. The special biomass color masterbatch is prepared from the following components: a plant coloring agent, cyclodextrin, a flame retardant, a modified polylactic acid, a plasticizer, an ultraviolet light absorber, an anti-aging agent, an inorganic filler and sodium stearate. As the color masterbatch, which is prepared by means of the modification treatment of a polylactic acid and cooperation between the modified polylactic acid and other components, is introduced into a degradable plastic, the comprehensive performances of the degradable plastic can be greatly improved, in particular, the tensile strength and the flame retardant property are obviously improved; moreover, the degradation performance of the degradable plastic is not influenced.
Description
本发明涉及塑料技术领域,具体为一种降解塑料专用生物质色母料。The invention relates to the technical field of plastics, in particular to a special biomass color masterbatch for degradable plastics.
塑料是一种生活中常用的一种材料,其因造价低廉被广泛使用与日常生活中,但是由于塑料本身特性使得塑料在不被使用后当作垃圾丢弃,很长时间内无法被自然降解回归至自然内,因此对自然造成较为严重的危害。Plastic is a kind of material commonly used in life. It is widely used in daily life because of its low cost. However, due to the characteristics of plastic itself, plastics are discarded as garbage after not being used, and cannot be naturally degraded and returned for a long time. into the nature, thus causing serious harm to nature.
而且随着人们生活水平的日益提高,生活质量大大改善,健康已成为了当前人们关系的话题,追求绿色产品和绿色消费已成为一种重要的需求。Moreover, with the improvement of people's living standards and the greatly improved quality of life, health has become a topic of current people's relationship, and the pursuit of green products and green consumption has become an important demand.
现有的降解塑料在加工时采用的色母粒依旧采用的传统的色母粒,生物降解性能较差,将其添加到降解塑料中使用后,会影响降解塑料的降解性能。The color masterbatch used in the processing of existing degradable plastics is still the traditional color masterbatch, which has poor biodegradability. After it is added to the degradable plastic for use, it will affect the degradation performance of the degradable plastic.
基于此,我们提出了一种降解塑料专用生物质色母料,希冀解决现有技术中的不足之处。Based on this, we propose a special biomass color masterbatch for degradable plastics, hoping to solve the deficiencies in the existing technology.
发明内容Contents of the invention
针对现有技术的不足,本发明提供了一种降解塑料专用生物质色母料。Aiming at the deficiencies of the prior art, the invention provides a special biomass color masterbatch for degradable plastics.
为实现上述的目的,本发明提供如下技术方案:To achieve the above object, the present invention provides the following technical solutions:
一种降解塑料专用生物质色母料,按重量份计由以下组分制成:植物染色剂22-26份、环糊精20-25份、阻燃剂1-3份、修饰聚乳酸35-40份、增塑剂1-3份、紫外线吸收剂1-2份、防老剂1.2-1.6份、无机填料5-7份、硬脂酸钠0.2-0.5份。A special biomass color masterbatch for degradable plastics, made of the following components in parts by weight: 22-26 parts of plant dyes, 20-25 parts of cyclodextrin, 1-3 parts of flame retardant, and 35 parts of modified polylactic acid -40 parts, 1-3 parts of plasticizer, 1-2 parts of ultraviolet absorber, 1.2-1.6 parts of anti-aging agent, 5-7 parts of inorganic filler, 0.2-0.5 parts of sodium stearate.
作为进一步的技术方案:所述修饰聚乳酸树脂制备方法为:As a further technical solution: the preparation method of the modified polylactic acid resin is:
(1)将聚乳酸添加到二甲苯中,调节温度值70℃,保温搅拌30min,得到均相溶液;(1) Add polylactic acid to xylene, adjust the temperature to 70°C, and keep stirring for 30 minutes to obtain a homogeneous solution;
(2)向步骤(1)中得到的均相溶液中添加聚天门冬氨酸溶液,调节温 度值50℃,保温搅拌40min,得到中间溶液;(2) Add polyaspartic acid solution to the homogeneous solution obtained in step (1), adjust the temperature value to 50°C, and keep stirring for 40min to obtain an intermediate solution;
(3)向步骤(2)中得到的中间溶液中添加甘油,以3000r/min转速搅拌40min,得到乳液;(3) Add glycerin to the intermediate solution obtained in step (2), stir with 3000r/min rotating speed for 40min, obtain emulsion;
(4)将步骤(3)得到的乳液进行冷冻相分离,待聚乳酸固化成微球后,进行洗涤,分离,得到改性聚乳酸。(4) The emulsion obtained in step (3) is subjected to freezing phase separation, and after the polylactic acid is solidified into microspheres, it is washed and separated to obtain modified polylactic acid.
作为进一步的技术方案,所述聚乳酸、二甲苯混合质量比为1∶12。As a further technical solution, the mixing mass ratio of polylactic acid and xylene is 1:12.
作为进一步的技术方案,所述均相溶液、聚天门冬氨酸溶液混合质量比为5∶1;As a further technical solution, the mixing mass ratio of the homogeneous solution and the polyaspartic acid solution is 5:1;
所述聚天门冬氨酸溶液质量分数为10%;The mass fraction of the polyaspartic acid solution is 10%;
所述中间溶液、甘油混合质量比为5∶2。The mixing mass ratio of the intermediate solution and glycerol is 5:2.
作为进一步的技术方案:所述植物染色剂为槐花提取物、苏木提取物、紫草提取物、冬青叶提取物、红花提取物、橡实提取物、乌桕叶提取物、石榴皮提取物、荷叶提取物、枫叶提取物、芦荟提取物、栗壳提取物中的一种或多种。As a further technical solution: the plant coloring agent is Sophora japonica extract, sumac extract, comfrey extract, wintergreen leaf extract, safflower extract, acorn extract, tallow leaf extract, pomegranate peel extract One or more of lotus leaf extract, maple leaf extract, aloe vera extract, chestnut shell extract.
作为进一步的技术方案:所述阻燃剂为氢氧化镁。As a further technical solution: the flame retardant is magnesium hydroxide.
作为进一步的技术方案,所述增塑剂为环氧大豆油。As a further technical solution, the plasticizer is epoxidized soybean oil.
作为进一步的技术方案,所述紫外线吸收剂为邻羟基苯甲酸苯酯。As a further technical solution, the ultraviolet absorber is phenyl o-hydroxybenzoate.
作为进一步的技术方案,所述防老剂为:N-苯基-α-苯胺;As a further technical solution, the anti-aging agent is: N-phenyl-α-aniline;
无机填料为硅藻土。The inorganic filler is diatomaceous earth.
一种降解塑料专用生物质色母料的制备方法,包括以下步骤:A preparation method of special biomass color masterbatch for degradable plastics, comprising the following steps:
(1)按重量份称取:植物染色剂、环糊精、阻燃剂、修饰聚乳酸、增塑剂、紫外线吸收剂、防老剂、无机填料、硬脂酸钠;(1) Take by weight: plant dyeing agent, cyclodextrin, flame retardant, modified polylactic acid, plasticizer, ultraviolet absorber, antioxidant, inorganic filler, sodium stearate;
(2)将上述原料添加到混料机中进行混料处理,以500r/min转速搅拌40min,得到混合初料;(2) Add the above-mentioned raw materials into a mixer for mixing, and stir for 40min at a speed of 500r/min to obtain a mixed raw material;
(3)将上述得到的混合初料添加到干燥机中,在60℃下干燥处理2小时, 得到干燥料;(3) Add the above-mentioned mixed raw material into a dryer, and dry it at 60° C. for 2 hours to obtain a dried material;
(4)将上述得到的干燥料添加到双螺杆挤出机中进行熔融挤出造粒,得到色母粒;(4) adding the dry material obtained above into a twin-screw extruder to carry out melt extrusion granulation to obtain color masterbatch;
其中,双螺杆挤出机的挤出温度为200℃。Wherein, the extrusion temperature of the twin-screw extruder is 200°C.
植物染色剂又称植物染料,是指利用自然界之花、草、树木、茎、叶、果实、种子、皮、根提取色素作为织物的染料。植物染色剂无毒无害,不会对人体健康造成伤害,同时,本发明中选用的植物染色成分还具有防虫、抗菌的作用,这是化学染料所不具备的。Plant dyes, also known as plant dyes, refer to dyes that use natural flowers, grasses, trees, stems, leaves, fruits, seeds, skins, and roots to extract pigments as fabrics. The plant dyeing agent is non-toxic and harmless, and will not cause harm to human health. At the same time, the plant dyeing components selected in the present invention also have insect-proof and antibacterial effects, which are not available in chemical dyes.
环糊精(Cyclodextrin,简称CD)是直链淀粉在由芽孢杆菌产生的环糊精葡萄糖基转移酶作用下生成的一系列环状低聚糖的总称,通常含有6~12个D-吡喃葡萄糖单元。其中研究得较多并且具有重要实际意义的是含有6、7、8个葡萄糖单元的分子,分别称为alpha-、beta-和gama-环糊精。根据X-线晶体衍射、红外光谱和核磁共振波谱分析的结果,确定构成环糊精分子的每个D(+)-吡喃葡萄糖都是椅式构象。各葡萄糖单元均以1,4-糖苷键结合成环。由于连接葡萄糖单元的糖苷键不能自由旋转,环糊精不是圆筒状分子而是略呈锥形的圆环。本发明通过利用环糊精独特的分子结构,将其引入到生物质色母粒制备中,能够有效的改善色母粒对于植物染色剂的吸附性能,增强对植物染色剂的承载量,从而提高其上色效果。Cyclodextrin (CD for short) is a general term for a series of cyclic oligosaccharides produced by amylose under the action of cyclodextrin glucosyltransferase produced by Bacillus, usually containing 6 to 12 D-pyrans glucose unit. Among them, molecules containing 6, 7, and 8 glucose units, which are studied more and have important practical significance, are called alpha-, beta-, and gama-cyclodextrins, respectively. According to the results of X-ray crystal diffraction, infrared spectrum and nuclear magnetic resonance spectrum analysis, it is determined that each D(+)-glucopyranose constituting the cyclodextrin molecule is in a chair conformation. Each glucose unit is joined by 1,4-glycosidic bonds to form a ring. Since the glycosidic bonds connecting the glucose units cannot rotate freely, cyclodextrins are not cylindrical molecules but slightly tapered rings. The invention utilizes the unique molecular structure of cyclodextrin and introduces it into the preparation of biomass color masterbatch, which can effectively improve the adsorption performance of the color masterbatch to the plant dyeing agent, enhance the carrying capacity of the plant dyeing agent, thereby increasing the Its coloring effect.
本发明通过对聚乳酸进行修饰处理,得到的修饰聚乳酸配合其他组分,制备的色母粒,将其引入到降解塑料中,能够大幅度的改善降解塑料的综合性能,尤其是拉伸强度和阻燃性能得到明显的提高,同时,还并不影响降解塑料的降解性能。In the present invention, by modifying polylactic acid, the obtained modified polylactic acid is combined with other components to prepare the color masterbatch, which is introduced into degradable plastics, which can greatly improve the comprehensive performance of degradable plastics, especially the tensile strength The flame retardancy and flame retardancy are significantly improved, and at the same time, the degradation performance of the degradable plastic is not affected.
与现有技术相比,本发明提供了一种降解塑料专用生物质色母料,具备以下有益效果:Compared with the prior art, the present invention provides a special biomass color masterbatch for degradable plastics, which has the following beneficial effects:
本发明通过对聚乳酸进行修饰处理,得到的修饰聚乳酸配合其他组分, 制备的色母粒,将其引入到降解塑料中,能够大幅度的改善降解塑料的综合性能,尤其是拉伸强度和阻燃性能得到明显的提高,同时,还并不影响降解塑料的降解性能。In the present invention, by modifying the polylactic acid, the obtained modified polylactic acid is combined with other components to prepare the color masterbatch, which is introduced into the degradable plastic, which can greatly improve the comprehensive performance of the degradable plastic, especially the tensile strength The flame retardancy and flame retardancy are significantly improved, and at the same time, the degradation performance of the degradable plastic is not affected.
图1为对比改性淀粉添加重量份对拉伸强度的影响图。Figure 1 is a graph showing the influence of the added weight of modified starch on the tensile strength.
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some, not all, embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
实施例1Example 1
一种降解塑料专用生物质色母料,按重量份计由以下组分制成:植物染色剂22份、环糊精20份、阻燃剂1份、修饰聚乳酸35份、增塑剂1份、紫外线吸收剂1份、防老剂1.2份、无机填料5份、硬脂酸钠0.2份。A special biomass color masterbatch for degradable plastics, made of the following components in parts by weight: 22 parts of vegetable dyes, 20 parts of cyclodextrin, 1 part of flame retardant, 35 parts of modified polylactic acid, and 1 part of plasticizer 1 part, 1 part of ultraviolet absorber, 1.2 parts of antioxidant, 5 parts of inorganic filler, 0.2 part of sodium stearate.
所述修饰聚乳酸树脂制备方法为:The preparation method of the modified polylactic acid resin is:
(1)将聚乳酸添加到二甲苯中,调节温度值70℃,保温搅拌30min,得到均相溶液;(1) Add polylactic acid to xylene, adjust the temperature to 70°C, and keep stirring for 30 minutes to obtain a homogeneous solution;
(2)向步骤(1)中得到的均相溶液中添加聚天门冬氨酸溶液,调节温度值50℃,保温搅拌40min,得到中间溶液;(2) Add polyaspartic acid solution to the homogeneous solution obtained in step (1), adjust the temperature value to 50° C., and keep stirring for 40 minutes to obtain an intermediate solution;
(3)向步骤(2)中得到的中间溶液中添加甘油,以3000r/min转速搅拌40min,得到乳液;(3) Add glycerin to the intermediate solution obtained in step (2), stir with 3000r/min rotating speed for 40min, obtain emulsion;
(4)将步骤(3)得到的乳液进行冷冻相分离,待聚乳酸固化成微球后,进行洗涤,分离,得到改性聚乳酸。(4) The emulsion obtained in step (3) is subjected to freezing phase separation, and after the polylactic acid is solidified into microspheres, it is washed and separated to obtain modified polylactic acid.
所述聚乳酸、二甲苯混合质量比为1∶12。The mixing mass ratio of polylactic acid and xylene is 1:12.
所述均相溶液、聚天门冬氨酸溶液混合质量比为5∶1;The mixing mass ratio of the homogeneous solution and the polyaspartic acid solution is 5:1;
所述聚天门冬氨酸溶液质量分数为10%;The mass fraction of the polyaspartic acid solution is 10%;
所述中间溶液、甘油混合质量比为5∶2。The mixing mass ratio of the intermediate solution and glycerin is 5:2.
所述植物染色剂为槐花提取物、苏木提取物、紫草提取物、冬青叶提取物、红花提取物、橡实提取物、乌桕叶提取物、石榴皮提取物、荷叶提取物、枫叶提取物、芦荟提取物、栗壳提取物中的一种或多种。The plant dyeing agent is Sophora japonica extract, sumac extract, comfrey extract, holly leaf extract, safflower extract, acorn extract, tallow leaf extract, pomegranate peel extract, lotus leaf extract , maple leaf extract, aloe extract, chestnut shell extract in one or more.
所述阻燃剂为氢氧化镁。The flame retardant is magnesium hydroxide.
所述增塑剂为环氧大豆油。Described plasticizer is epoxidized soybean oil.
所述紫外线吸收剂为邻羟基苯甲酸苯酯。The ultraviolet absorber is phenyl o-hydroxybenzoate.
所述防老剂为:N-苯基-α-苯胺;The anti-aging agent is: N-phenyl-α-aniline;
无机填料为硅藻土。The inorganic filler is diatomaceous earth.
一种降解塑料专用生物质色母料的制备方法,包括以下步骤:A preparation method of special biomass color masterbatch for degradable plastics, comprising the following steps:
(1)按重量份称取:植物染色剂、环糊精、阻燃剂、修饰聚乳酸、增塑剂、紫外线吸收剂、防老剂、无机填料、硬脂酸钠;(1) Take by weight: plant dyeing agent, cyclodextrin, flame retardant, modified polylactic acid, plasticizer, ultraviolet absorber, antioxidant, inorganic filler, sodium stearate;
(2)将上述原料添加到混料机中进行混料处理,以500r/min转速搅拌40min,得到混合初料;(2) Add the above-mentioned raw materials into a mixer for mixing, and stir for 40min at a speed of 500r/min to obtain a mixed raw material;
(3)将上述得到的混合初料添加到干燥机中,在60℃下干燥处理2小时,得到干燥料;(3) adding the above-mentioned mixed primary material into a dryer, and drying at 60° C. for 2 hours to obtain a dried material;
(4)将上述得到的干燥料添加到双螺杆挤出机中进行熔融挤出造粒,得到色母粒;(4) adding the dry material obtained above into a twin-screw extruder to carry out melt extrusion granulation to obtain color masterbatch;
其中,双螺杆挤出机的挤出温度为200℃。Wherein, the extrusion temperature of the twin-screw extruder is 200°C.
实施例2Example 2
一种降解塑料专用生物质色母料,按重量份计由以下组分制成:植物染色剂23份、环糊精24份、阻燃剂2份、修饰聚乳酸37份、增塑剂1.8份、紫外线吸收剂1.6份、防老剂1.4份、无机填料6.8份、硬脂酸钠0.35份。A special biomass color masterbatch for degradable plastics, made of the following components in parts by weight: 23 parts of vegetable dyes, 24 parts of cyclodextrin, 2 parts of flame retardants, 37 parts of modified polylactic acid, and 1.8 parts of plasticizers parts, 1.6 parts of ultraviolet absorbers, 1.4 parts of antioxidants, 6.8 parts of inorganic fillers, and 0.35 parts of sodium stearate.
所述修饰聚乳酸树脂制备方法为:The preparation method of the modified polylactic acid resin is:
(1)将聚乳酸添加到二甲苯中,调节温度值70℃,保温搅拌30min,得到均相溶液;(1) Add polylactic acid to xylene, adjust the temperature to 70°C, and keep stirring for 30 minutes to obtain a homogeneous solution;
(2)向步骤(1)中得到的均相溶液中添加聚天门冬氨酸溶液,调节温度值50℃,保温搅拌40min,得到中间溶液;(2) Add polyaspartic acid solution to the homogeneous solution obtained in step (1), adjust the temperature value to 50° C., and keep stirring for 40 minutes to obtain an intermediate solution;
(3)向步骤(2)中得到的中间溶液中添加甘油,以3000r/min转速搅拌40min,得到乳液;(3) Add glycerin to the intermediate solution obtained in step (2), stir with 3000r/min rotating speed for 40min, obtain emulsion;
(4)将步骤(3)得到的乳液进行冷冻相分离,待聚乳酸固化成微球后,进行洗涤,分离,得到改性聚乳酸。(4) The emulsion obtained in step (3) is subjected to freezing phase separation, and after the polylactic acid is solidified into microspheres, it is washed and separated to obtain modified polylactic acid.
所述聚乳酸、二甲苯混合质量比为1∶12。The mixing mass ratio of polylactic acid and xylene is 1:12.
所述均相溶液、聚天门冬氨酸溶液混合质量比为5∶1;The mixing mass ratio of the homogeneous solution and the polyaspartic acid solution is 5:1;
所述聚天门冬氨酸溶液质量分数为10%;The mass fraction of the polyaspartic acid solution is 10%;
所述中间溶液、甘油混合质量比为5∶2。The mixing mass ratio of the intermediate solution and glycerol is 5:2.
所述植物染色剂为槐花提取物、苏木提取物、紫草提取物、冬青叶提取物、红花提取物、橡实提取物、乌桕叶提取物、石榴皮提取物、荷叶提取物、枫叶提取物、芦荟提取物、栗壳提取物中的一种或多种。The plant dyeing agent is Sophora japonica extract, sumac extract, comfrey extract, holly leaf extract, safflower extract, acorn extract, tallow leaf extract, pomegranate peel extract, lotus leaf extract , maple leaf extract, aloe extract, chestnut shell extract in one or more.
所述阻燃剂为氢氧化镁。The flame retardant is magnesium hydroxide.
所述增塑剂为环氧大豆油。Described plasticizer is epoxidized soybean oil.
所述紫外线吸收剂为邻羟基苯甲酸苯酯。The ultraviolet absorber is phenyl o-hydroxybenzoate.
所述防老剂为:N-苯基-α-苯胺;The anti-aging agent is: N-phenyl-α-aniline;
无机填料为硅藻土。The inorganic filler is diatomaceous earth.
一种降解塑料专用生物质色母料的制备方法,包括以下步骤:A preparation method of special biomass color masterbatch for degradable plastics, comprising the following steps:
(1)按重量份称取:植物染色剂、环糊精、阻燃剂、修饰聚乳酸、增塑剂、紫外线吸收剂、防老剂、无机填料、硬脂酸钠;(1) Take by weight: plant dyeing agent, cyclodextrin, flame retardant, modified polylactic acid, plasticizer, ultraviolet absorber, antioxidant, inorganic filler, sodium stearate;
(2)将上述原料添加到混料机中进行混料处理,以500r/min转速搅拌40min,得到混合初料;(2) Add the above-mentioned raw materials into a mixer for mixing, and stir for 40min at a speed of 500r/min to obtain a mixed raw material;
(3)将上述得到的混合初料添加到干燥机中,在60℃下干燥处理2小时,得到干燥料;(3) adding the above-mentioned mixed primary material into a dryer, and drying at 60° C. for 2 hours to obtain a dried material;
(4)将上述得到的干燥料添加到双螺杆挤出机中进行熔融挤出造粒,得到色母粒;(4) adding the dry material obtained above into a twin-screw extruder to carry out melt extrusion granulation to obtain color masterbatch;
其中,双螺杆挤出机的挤出温度为200℃。Wherein, the extrusion temperature of the twin-screw extruder is 200°C.
实施例3Example 3
一种降解塑料专用生物质色母料,按重量份计由以下组分制成:植物染色剂23.5份、环糊精22.5份、阻燃剂2.1份、修饰聚乳酸38份、增塑剂1.3份、紫外线吸收剂1.4份、防老剂1.3份、无机填料6.5份、硬脂酸钠0.2份。A special biomass color masterbatch for degradable plastics, made of the following components in parts by weight: 23.5 parts of vegetable dyes, 22.5 parts of cyclodextrin, 2.1 parts of flame retardants, 38 parts of modified polylactic acid, and 1.3 parts of plasticizers parts, 1.4 parts of ultraviolet absorbers, 1.3 parts of antioxidants, 6.5 parts of inorganic fillers, and 0.2 parts of sodium stearate.
所述修饰聚乳酸树脂制备方法为:The preparation method of the modified polylactic acid resin is:
(1)将聚乳酸添加到二甲苯中,调节温度值70℃,保温搅拌30min,得到均相溶液;(1) Add polylactic acid to xylene, adjust the temperature to 70°C, and keep stirring for 30 minutes to obtain a homogeneous solution;
(2)向步骤(1)中得到的均相溶液中添加聚天门冬氨酸溶液,调节温度值50℃,保温搅拌40min,得到中间溶液;(2) Add polyaspartic acid solution to the homogeneous solution obtained in step (1), adjust the temperature value to 50° C., and keep stirring for 40 minutes to obtain an intermediate solution;
(3)向步骤(2)中得到的中间溶液中添加甘油,以3000r/min转速搅拌40min,得到乳液;(3) Add glycerin to the intermediate solution obtained in step (2), stir with 3000r/min rotating speed for 40min, obtain emulsion;
(4)将步骤(3)得到的乳液进行冷冻相分离,待聚乳酸固化成微球后,进行洗涤,分离,得到改性聚乳酸。(4) The emulsion obtained in step (3) is subjected to freezing phase separation, and after the polylactic acid is solidified into microspheres, it is washed and separated to obtain modified polylactic acid.
所述聚乳酸、二甲苯混合质量比为1∶12。The mixing mass ratio of polylactic acid and xylene is 1:12.
所述均相溶液、聚天门冬氨酸溶液混合质量比为5∶1;The mixing mass ratio of the homogeneous solution and the polyaspartic acid solution is 5:1;
所述聚天门冬氨酸溶液质量分数为10%;The mass fraction of the polyaspartic acid solution is 10%;
所述中间溶液、甘油混合质量比为5∶2。The mixing mass ratio of the intermediate solution and glycerin is 5:2.
所述植物染色剂为槐花提取物、苏木提取物、紫草提取物、冬青叶提取物、红花提取物、橡实提取物、乌桕叶提取物、石榴皮提取物、荷叶提取物、 枫叶提取物、芦荟提取物、栗壳提取物中的一种或多种。The plant dyeing agent is Sophora japonica extract, sumac extract, comfrey extract, holly leaf extract, safflower extract, acorn extract, tallow leaf extract, pomegranate peel extract, lotus leaf extract , maple leaf extract, aloe extract, chestnut shell extract in one or more.
所述阻燃剂为氢氧化镁。The flame retardant is magnesium hydroxide.
所述增塑剂为环氧大豆油。Described plasticizer is epoxidized soybean oil.
所述紫外线吸收剂为邻羟基苯甲酸苯酯。The ultraviolet absorber is phenyl o-hydroxybenzoate.
所述防老剂为:N-苯基α苯胺;The anti-aging agent is: N-phenyl α aniline;
无机填料为硅藻土。The inorganic filler is diatomaceous earth.
一种降解塑料专用生物质色母料的制备方法,包括以下步骤:A preparation method of special biomass color masterbatch for degradable plastics, comprising the following steps:
(1)按重量份称取:植物染色剂、环糊精、阻燃剂、修饰聚乳酸、增塑剂、紫外线吸收剂、防老剂、无机填料、硬脂酸钠;(1) Take by weight: plant dyeing agent, cyclodextrin, flame retardant, modified polylactic acid, plasticizer, ultraviolet absorber, antioxidant, inorganic filler, sodium stearate;
(2)将上述原料添加到混料机中进行混料处理,以500r/min转速搅拌40min,得到混合初料;(2) Add the above-mentioned raw materials into a mixer for mixing, and stir for 40min at a speed of 500r/min to obtain a mixed raw material;
(3)将上述得到的混合初料添加到干燥机中,在60℃下干燥处理2小时,得到干燥料;(3) adding the above-mentioned mixed primary material into a dryer, and drying at 60° C. for 2 hours to obtain a dried material;
(4)将上述得到的干燥料添加到双螺杆挤出机中进行熔融挤出造粒,得到色母粒;(4) adding the dry material obtained above into a twin-screw extruder to carry out melt extrusion granulation to obtain color masterbatch;
其中,双螺杆挤出机的挤出温度为200℃。Wherein, the extrusion temperature of the twin-screw extruder is 200°C.
实施例4Example 4
一种降解塑料专用生物质色母料,按重量份计由以下组分制成:植物染色剂24份、环糊精22份、阻燃剂2.2份、修饰聚乳酸37份、增塑剂2.5份、紫外线吸收剂1.8份、防老剂1.4份、无机填料5.5份、硬脂酸钠0.3份。A special biomass color masterbatch for degradable plastics, made of the following components in parts by weight: 24 parts of vegetable dyes, 22 parts of cyclodextrin, 2.2 parts of flame retardants, 37 parts of modified polylactic acid, 2.5 parts of plasticizers parts, 1.8 parts of ultraviolet absorbers, 1.4 parts of antioxidants, 5.5 parts of inorganic fillers, and 0.3 parts of sodium stearate.
所述修饰聚乳酸树脂制备方法为:The preparation method of the modified polylactic acid resin is:
(1)将聚乳酸添加到二甲苯中,调节温度值70℃,保温搅拌30min,得到均相溶液;(1) Add polylactic acid to xylene, adjust the temperature to 70°C, and keep stirring for 30 minutes to obtain a homogeneous solution;
(2)向步骤(1)中得到的均相溶液中添加聚天门冬氨酸溶液,调节温度值50℃,保温搅拌40min,得到中间溶液;(2) Add polyaspartic acid solution to the homogeneous solution obtained in step (1), adjust the temperature value to 50° C., and keep stirring for 40 minutes to obtain an intermediate solution;
(3)向步骤(2)中得到的中间溶液中添加甘油,以3000r/min转速搅拌40min,得到乳液;(3) Add glycerin to the intermediate solution obtained in step (2), stir with 3000r/min rotating speed for 40min, obtain emulsion;
(4)将步骤(3)得到的乳液进行冷冻相分离,待聚乳酸固化成微球后,进行洗涤,分离,得到改性聚乳酸。(4) The emulsion obtained in step (3) is subjected to freezing phase separation, and after the polylactic acid is solidified into microspheres, it is washed and separated to obtain modified polylactic acid.
所述聚乳酸、二甲苯混合质量比为1∶12。The mixing mass ratio of polylactic acid and xylene is 1:12.
所述均相溶液、聚天门冬氨酸溶液混合质量比为5∶1;The mixing mass ratio of the homogeneous solution and the polyaspartic acid solution is 5:1;
所述聚天门冬氨酸溶液质量分数为10%;The mass fraction of the polyaspartic acid solution is 10%;
所述中间溶液、甘油混合质量比为5∶2。The mixing mass ratio of the intermediate solution and glycerol is 5:2.
所述植物染色剂为槐花提取物、苏木提取物、紫草提取物、冬青叶提取物、红花提取物、橡实提取物、乌桕叶提取物、石榴皮提取物、荷叶提取物、枫叶提取物、芦荟提取物、栗壳提取物中的一种或多种。The plant dyeing agent is Sophora japonica extract, sumac extract, comfrey extract, holly leaf extract, safflower extract, acorn extract, tallow leaf extract, pomegranate peel extract, lotus leaf extract , maple leaf extract, aloe extract, chestnut shell extract in one or more.
所述阻燃剂为氢氧化镁。The flame retardant is magnesium hydroxide.
所述增塑剂为环氧大豆油。Described plasticizer is epoxidized soybean oil.
所述紫外线吸收剂为邻羟基苯甲酸苯酯。The ultraviolet absorber is phenyl o-hydroxybenzoate.
所述防老剂为:N-苯基-α-苯胺;The anti-aging agent is: N-phenyl-α-aniline;
无机填料为硅藻土。The inorganic filler is diatomaceous earth.
一种降解塑料专用生物质色母料的制备方法,包括以下步骤:A preparation method of special biomass color masterbatch for degradable plastics, comprising the following steps:
(1)按重量份称取:植物染色剂、环糊精、阻燃剂、修饰聚乳酸、增塑剂、紫外线吸收剂、防老剂、无机填料、硬脂酸钠;(1) Take by weight: plant dyeing agent, cyclodextrin, flame retardant, modified polylactic acid, plasticizer, ultraviolet absorber, antioxidant, inorganic filler, sodium stearate;
(2)将上述原料添加到混料机中进行混料处理,以500r/min转速搅拌40min,得到混合初料;(2) Add the above-mentioned raw materials into a mixer for mixing, and stir for 40min at a speed of 500r/min to obtain a mixed raw material;
(3)将上述得到的混合初料添加到干燥机中,在60℃下干燥处理2小时,得到干燥料;(3) adding the above-mentioned mixed primary material into a dryer, and drying at 60° C. for 2 hours to obtain a dried material;
(4)将上述得到的干燥料添加到双螺杆挤出机中进行熔融挤出造粒,得到色母粒;(4) adding the dry material obtained above into a twin-screw extruder to carry out melt extrusion granulation to obtain color masterbatch;
其中,双螺杆挤出机的挤出温度为200℃。Wherein, the extrusion temperature of the twin-screw extruder is 200°C.
实施例5Example 5
一种降解塑料专用生物质色母料,按重量份计由以下组分制成:植物染色剂25份、环糊精24份、阻燃剂2份、修饰聚乳酸38份、增塑剂2份、紫外线吸收剂1.5份、防老剂1.5份、无机填料6份、硬脂酸钠0.4份。A special biomass color masterbatch for degradable plastics, made of the following components in parts by weight: 25 parts of vegetable dyes, 24 parts of cyclodextrin, 2 parts of flame retardants, 38 parts of modified polylactic acid, 2 parts of plasticizers 1.5 parts, 1.5 parts of ultraviolet absorber, 1.5 parts of antioxidant, 6 parts of inorganic filler, 0.4 part of sodium stearate.
所述修饰聚乳酸树脂制备方法为:The preparation method of the modified polylactic acid resin is:
(1)将聚乳酸添加到二甲苯中,调节温度值70℃,保温搅拌30min,得到均相溶液;(1) Add polylactic acid to xylene, adjust the temperature to 70°C, and keep stirring for 30 minutes to obtain a homogeneous solution;
(2)向步骤(1)中得到的均相溶液中添加聚天门冬氨酸溶液,调节温度值50℃,保温搅拌40min,得到中间溶液;(2) Add polyaspartic acid solution to the homogeneous solution obtained in step (1), adjust the temperature value to 50° C., and keep stirring for 40 minutes to obtain an intermediate solution;
(3)向步骤(2)中得到的中间溶液中添加甘油,以3000r/min转速搅拌40min,得到乳液;(3) Add glycerin to the intermediate solution obtained in step (2), stir with 3000r/min rotating speed for 40min, obtain emulsion;
(4)将步骤(3)得到的乳液进行冷冻相分离,待聚乳酸固化成微球后,进行洗涤,分离,得到改性聚乳酸。(4) The emulsion obtained in step (3) is subjected to freezing phase separation, and after the polylactic acid is solidified into microspheres, it is washed and separated to obtain modified polylactic acid.
所述聚乳酸、二甲苯混合质量比为1∶12。The mixing mass ratio of polylactic acid and xylene is 1:12.
所述均相溶液、聚天门冬氨酸溶液混合质量比为5∶1;The mixing mass ratio of the homogeneous solution and the polyaspartic acid solution is 5:1;
所述聚天门冬氨酸溶液质量分数为10%;The mass fraction of the polyaspartic acid solution is 10%;
所述中间溶液、甘油混合质量比为5∶2。The mixing mass ratio of the intermediate solution and glycerin is 5:2.
所述植物染色剂为槐花提取物、苏木提取物、紫草提取物、冬青叶提取物、红花提取物、橡实提取物、乌桕叶提取物、石榴皮提取物、荷叶提取物、枫叶提取物、芦荟提取物、栗壳提取物中的一种或多种。The plant dyeing agent is Sophora japonica extract, sumac extract, comfrey extract, holly leaf extract, safflower extract, acorn extract, tallow leaf extract, pomegranate peel extract, lotus leaf extract , maple leaf extract, aloe extract, chestnut shell extract in one or more.
所述阻燃剂为氢氧化镁。The flame retardant is magnesium hydroxide.
所述增塑剂为环氧大豆油。Described plasticizer is epoxidized soybean oil.
所述紫外线吸收剂为邻羟基苯甲酸苯酯。The ultraviolet absorber is phenyl o-hydroxybenzoate.
所述防老剂为:N-苯基-α-苯胺;The anti-aging agent is: N-phenyl-α-aniline;
无机填料为硅藻土。The inorganic filler is diatomaceous earth.
一种降解塑料专用生物质色母料的制备方法,包括以下步骤:A preparation method of special biomass color masterbatch for degradable plastics, comprising the following steps:
(1)按重量份称取:植物染色剂、环糊精、阻燃剂、修饰聚乳酸、增塑剂、紫外线吸收剂、防老剂、无机填料、硬脂酸钠;(1) Take by weight: plant dyeing agent, cyclodextrin, flame retardant, modified polylactic acid, plasticizer, ultraviolet absorber, antioxidant, inorganic filler, sodium stearate;
(2)将上述原料添加到混料机中进行混料处理,以500r/min转速搅拌40min,得到混合初料;(2) Add the above-mentioned raw materials into a mixer for mixing, and stir for 40min at a speed of 500r/min to obtain a mixed raw material;
(3)将上述得到的混合初料添加到干燥机中,在60℃下干燥处理2小时,得到干燥料;(3) adding the above-mentioned mixed primary material into a dryer, and drying at 60° C. for 2 hours to obtain a dried material;
(4)将上述得到的干燥料添加到双螺杆挤出机中进行熔融挤出造粒,得到色母粒;(4) adding the dry material obtained above into a twin-screw extruder to carry out melt extrusion granulation to obtain color masterbatch;
其中,双螺杆挤出机的挤出温度为200℃。Wherein, the extrusion temperature of the twin-screw extruder is 200°C.
实施例6Example 6
一种降解塑料专用生物质色母料,按重量份计由以下组分制成:植物染色剂26份、环糊精25份、阻燃剂3份、修饰聚乳酸40份、增塑剂3份、紫外线吸收剂2份、防老剂1.6份、无机填料7份、硬脂酸钠0.5份。A special biomass color masterbatch for degradable plastics, made of the following components in parts by weight: 26 parts of vegetable dyes, 25 parts of cyclodextrin, 3 parts of flame retardants, 40 parts of modified polylactic acid, and 3 parts of plasticizers 2 parts, 2 parts of ultraviolet absorber, 1.6 parts of antioxidant, 7 parts of inorganic filler, 0.5 part of sodium stearate.
所述修饰聚乳酸树脂制备方法为:The preparation method of the modified polylactic acid resin is:
(1)将聚乳酸添加到二甲苯中,调节温度值70℃,保温搅拌30min,得到均相溶液;(1) Add polylactic acid to xylene, adjust the temperature to 70°C, and keep stirring for 30 minutes to obtain a homogeneous solution;
(2)向步骤(1)中得到的均相溶液中添加聚天门冬氨酸溶液,调节温度值50℃,保温搅拌40min,得到中间溶液;(2) Add polyaspartic acid solution to the homogeneous solution obtained in step (1), adjust the temperature value to 50° C., and keep stirring for 40 minutes to obtain an intermediate solution;
(3)向步骤(2)中得到的中间溶液中添加甘油,以3000r/min转速搅拌40min,得到乳液;(3) Add glycerin to the intermediate solution obtained in step (2), stir with 3000r/min rotating speed for 40min, obtain emulsion;
(4)将步骤(3)得到的乳液进行冷冻相分离,待聚乳酸固化成微球后,进行洗涤,分离,得到改性聚乳酸。(4) The emulsion obtained in step (3) is subjected to freezing phase separation, and after the polylactic acid is solidified into microspheres, it is washed and separated to obtain modified polylactic acid.
所述聚乳酸、二甲苯混合质量比为1∶12。The mixing mass ratio of polylactic acid and xylene is 1:12.
所述均相溶液、聚天门冬氨酸溶液混合质量比为5∶1;The mixing mass ratio of the homogeneous solution and the polyaspartic acid solution is 5:1;
所述聚天门冬氨酸溶液质量分数为10%;The mass fraction of the polyaspartic acid solution is 10%;
所述中间溶液、甘油混合质量比为5∶2。The mixing mass ratio of the intermediate solution and glycerin is 5:2.
所述植物染色剂为槐花提取物、苏木提取物、紫草提取物、冬青叶提取物、红花提取物、橡实提取物、乌桕叶提取物、石榴皮提取物、荷叶提取物、枫叶提取物、芦荟提取物、栗壳提取物中的一种或多种。The plant dyeing agent is Sophora japonica extract, sumac extract, comfrey extract, holly leaf extract, safflower extract, acorn extract, tallow leaf extract, pomegranate peel extract, lotus leaf extract , maple leaf extract, aloe extract, chestnut shell extract in one or more.
所述阻燃剂为氢氧化镁。The flame retardant is magnesium hydroxide.
所述增塑剂为环氧大豆油。Described plasticizer is epoxidized soybean oil.
所述紫外线吸收剂为邻羟基苯甲酸苯酯。The ultraviolet absorber is phenyl o-hydroxybenzoate.
所述防老剂为:N-苯基-α-苯胺;The anti-aging agent is: N-phenyl-α-aniline;
无机填料为硅藻土。The inorganic filler is diatomaceous earth.
一种降解塑料专用生物质色母料的制备方法,包括以下步骤:A preparation method of special biomass color masterbatch for degradable plastics, comprising the following steps:
(1)按重量份称取:植物染色剂、环糊精、阻燃剂、修饰聚乳酸、增塑剂、紫外线吸收剂、防老剂、无机填料、硬脂酸钠;(1) Take by weight: plant dyeing agent, cyclodextrin, flame retardant, modified polylactic acid, plasticizer, ultraviolet absorber, antioxidant, inorganic filler, sodium stearate;
(2)将上述原料添加到混料机中进行混料处理,以500r/min转速搅拌40min,得到混合初料;(2) Add the above-mentioned raw materials into a mixer for mixing, and stir for 40min at a speed of 500r/min to obtain a mixed raw material;
(3)将上述得到的混合初料添加到干燥机中,在60℃下干燥处理2小时,得到干燥料;(3) adding the above-mentioned mixed primary material into a dryer, and drying at 60° C. for 2 hours to obtain a dried material;
(4)将上述得到的干燥料添加到双螺杆挤出机中进行熔融挤出造粒,得到色母粒;(4) adding the dry material obtained above into a twin-screw extruder to carry out melt extrusion granulation to obtain color masterbatch;
其中,双螺杆挤出机的挤出温度为200℃。Wherein, the extrusion temperature of the twin-screw extruder is 200°C.
以申请号201310360960.4一种可降解塑料及其制备方法,制备的可降解塑料为试样,按10∶1质量比例分别添加实施例与对比例色母粒,采用其公开的制备方法进行制备,用万能试验机测试样条的力学性能,根据GB/T1040-1979标准在速率为20mm/min条件下,测量材料的拉伸强度:Using application number 201310360960.4, a degradable plastic and its preparation method, the prepared degradable plastic was used as a sample, and the color masterbatches of the examples and the comparative examples were added in a mass ratio of 10:1, and prepared by the disclosed preparation method. The universal testing machine tests the mechanical properties of the sample, and measures the tensile strength of the material at a rate of 20mm/min according to the GB/T1040-1979 standard:
表1Table 1
the | 拉伸强度/MPaTensile strength/MPa |
实施例1Example 1 | 30.130.1 |
实施例2Example 2 | 30.230.2 |
实施例3Example 3 | 30.530.5 |
实施例4Example 4 | 30.930.9 |
实施例5Example 5 | 29.829.8 |
实施例6Example 6 | 30.430.4 |
对比例1Comparative example 1 | 28.428.4 |
对比例1:与实施例1区别为将修饰聚乳酸树脂替换未改性处理的聚乳酸;Comparative Example 1: The difference from Example 1 is that the modified polylactic acid resin is replaced by the unmodified polylactic acid;
由表1可以看出,本发明制备的色母粒引入到降解塑料中,能够一定程度上改善提高其力学性能,尤其是拉伸强度,具有明显的提高。It can be seen from Table 1 that the introduction of the masterbatch prepared by the present invention into degradable plastics can improve its mechanical properties to a certain extent, especially the tensile strength, which has a significant increase.
进一步实验,降解性:用ASTM·D5338-92方法测定塑料在受控堆肥条件下需氧生物降解率:Further experiments, degradability: use ASTM D5338-92 method to determine the aerobic biodegradation rate of plastics under controlled composting conditions:
表2Table 2
the | 需氧生物降解率%Aerobic biodegradation rate% |
实施例1Example 1 | 24.624.6 |
实施例2Example 2 | 24.824.8 |
实施例3Example 3 | 24.124.1 |
实施例4Example 4 | 24.024.0 |
实施例5Example 5 | 24.524.5 |
实施例6Example 6 | 24.624.6 |
对比例1Comparative example 1 | 22.722.7 |
对比例1:与实施例1区别为将修饰聚乳酸树脂替换未改性处理的聚乳酸;Comparative Example 1: The difference from Example 1 is that the modified polylactic acid resin is replaced by the unmodified polylactic acid;
由表2可以看出,本发明制备的生物质色母粒引入到降解塑料中,能够进一步的改善其降解性能。It can be seen from Table 2 that the introduction of the biomass color masterbatch prepared by the present invention into degradable plastics can further improve its degradation performance.
进一步实验,阻燃性能按UL94标准规定的测试方法进行垂直燃烧测试:For further experiments, the flame retardant performance was tested according to the test method specified in the UL94 standard:
表3table 3
the | 阻燃性能/级Flame retardant performance/grade |
实施例1Example 1 | V-1V-1 |
实施例2Example 2 | V-1V-1 |
实施例3Example 3 | V-1V-1 |
实施例4Example 4 | V-1V-1 |
实施例5Example 5 | V-1V-1 |
实施例6Example 6 | V-1V-1 |
空白对照组Blank control group | V-4V-4 |
空白对照组:申请号201310360960.4一种可降解塑料及其制备方法制备的塑料;Blank control group: application number 201310360960.4, a degradable plastic and a plastic prepared by its preparation method;
由表3可以看出,本发明制备的生物质色母粒具有一定的阻燃性能。It can be seen from Table 3 that the biomass color masterbatch prepared by the present invention has certain flame retardant properties.
以实施例1为基础试样,申请号201310360960.4一种可降解塑料及其制备方法制备的塑料为试验试样,对比实施例不同添加比例对降解塑料拉伸强度的影响。Taking Example 1 as the basic sample, application number 201310360960.4, a degradable plastic and a plastic prepared by its preparation method, as the test sample, compare the effects of different addition ratios of Examples on the tensile strength of the degradable plastic.
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。Although the embodiments of the present invention have been shown and described, those skilled in the art can understand that various changes, modifications and substitutions can be made to these embodiments without departing from the principle and spirit of the present invention. and modifications, the scope of the invention is defined by the appended claims and their equivalents.
Claims (10)
- 一种降解塑料专用生物质色母料,其特征在于,按重量份计由以下组分制成:植物染色剂22-26份、环糊精20-25份、阻燃剂1-3份、修饰聚乳酸35-40份、增塑剂1-3份、紫外线吸收剂1-2份、防老剂1.2-1.6份、无机填料5-7份、硬脂酸钠0.2-0.5份。A special biomass color masterbatch for degradable plastics, characterized in that it is made of the following components in parts by weight: 22-26 parts of plant dyeing agent, 20-25 parts of cyclodextrin, 1-3 parts of flame retardant, 35-40 parts of modified polylactic acid, 1-3 parts of plasticizer, 1-2 parts of ultraviolet absorber, 1.2-1.6 parts of anti-aging agent, 5-7 parts of inorganic filler, 0.2-0.5 part of sodium stearate.
- 根据权利要求1所述的一种降解塑料专用生物质色母料,其特征在于:所述修饰聚乳酸树脂制备方法为:A special biomass color masterbatch for degradable plastics according to claim 1, characterized in that: the preparation method of the modified polylactic acid resin is:(1)将聚乳酸添加到二甲苯中,调节温度值70℃,保温搅拌30min,得到均相溶液;(1) Add polylactic acid to xylene, adjust the temperature to 70°C, and keep stirring for 30 minutes to obtain a homogeneous solution;(2)向步骤(1)中得到的均相溶液中添加聚天门冬氨酸溶液,调节温度值50℃,保温搅拌40min,得到中间溶液;(2) Add polyaspartic acid solution to the homogeneous solution obtained in step (1), adjust the temperature value to 50° C., and keep stirring for 40 minutes to obtain an intermediate solution;(3)向步骤(2)中得到的中间溶液中添加甘油,以3000r/min转速搅拌40min,得到乳液;(3) Add glycerin to the intermediate solution obtained in step (2), stir with 3000r/min rotating speed for 40min, obtain emulsion;(4)将步骤(3)得到的乳液进行冷冻相分离,待聚乳酸固化成微球后,进行洗涤,分离,得到改性聚乳酸。(4) The emulsion obtained in step (3) is subjected to freezing phase separation, and after the polylactic acid is solidified into microspheres, it is washed and separated to obtain modified polylactic acid.
- 根据权利要求2所述的一种降解塑料专用生物质色母料,其特征在于,所述聚乳酸、二甲苯混合质量比为1∶12。The special biomass color masterbatch for degradable plastics according to claim 2, characterized in that the mixing mass ratio of polylactic acid and xylene is 1:12.
- 根据权利要求2所述的一种降解塑料专用生物质色母料,其特征在于,所述均相溶液、聚天门冬氨酸溶液混合质量比为5∶1;A special biomass color masterbatch for degradable plastics according to claim 2, characterized in that the mixing mass ratio of the homogeneous solution and the polyaspartic acid solution is 5:1;所述聚天门冬氨酸溶液质量分数为10%;The mass fraction of the polyaspartic acid solution is 10%;所述中间溶液、甘油混合质量比为5∶2。The mixing mass ratio of the intermediate solution and glycerol is 5:2.
- 根据权利要求1所述的一种降解塑料专用生物质色母料,其特征在于:所述植物染色剂为槐花提取物、苏木提取物、紫草提取物、冬青叶提取物、红花提取物、橡实提取物、乌桕叶提取物、石榴皮提取物、荷叶提取物、枫叶提取物、芦荟提取物、栗壳提取物中的一种或多种。A special biomass color masterbatch for degradable plastics according to claim 1, characterized in that: the plant coloring agent is Sophora japonica extract, sumac extract, comfrey extract, holly leaf extract, safflower Extract, acorn extract, tallow tree leaf extract, pomegranate bark extract, lotus leaf extract, maple leaf extract, aloe extract, chestnut shell extract.
- 根据权利要求1所述的一种降解塑料专用生物质色母料,其特征在于: 所述阻燃剂为氢氧化镁。The special biomass color masterbatch for degradable plastics according to claim 1, characterized in that: the flame retardant is magnesium hydroxide.
- 根据权利要求1所述的一种降解塑料专用生物质色母料,其特征在于,所述增塑剂为环氧大豆油。The special biomass color masterbatch for degradable plastics according to claim 1, wherein the plasticizer is epoxidized soybean oil.
- 根据权利要求1所述的一种降解塑料专用生物质色母料,其特征在于,所述紫外线吸收剂为邻羟基苯甲酸苯酯。The special biomass color masterbatch for degradable plastics according to claim 1, wherein the ultraviolet absorber is phenyl o-hydroxybenzoate.
- 根据权利要求1所述的一种降解塑料专用生物质色母料,其特征在于,所述防老剂为:N-苯基-α-苯胺;A special biomass color masterbatch for degradable plastics according to claim 1, wherein the anti-aging agent is: N-phenyl-α-aniline;无机填料为硅藻土。The inorganic filler is diatomaceous earth.
- 根据权利要求1所述的一种降解塑料专用生物质色母料的制备方法,其特征在于,包括以下步骤:The preparation method of a special biomass color masterbatch for degradable plastics according to claim 1, characterized in that it comprises the following steps:(1)按重量份称取:植物染色剂、环糊精、阻燃剂、修饰聚乳酸、增塑剂、紫外线吸收剂、防老剂、无机填料、硬脂酸钠;(1) Take by weight: plant dyeing agent, cyclodextrin, flame retardant, modified polylactic acid, plasticizer, ultraviolet absorber, antioxidant, inorganic filler, sodium stearate;(2)将上述原料添加到混料机中进行混料处理,以500r/min转速搅拌40min,得到混合初料;(2) Add the above-mentioned raw materials into a mixer for mixing, and stir for 40min at a speed of 500r/min to obtain a mixed raw material;(3)将上述得到的混合初料添加到干燥机中,在60℃下干燥处理2小时,得到干燥料;(3) adding the above-mentioned mixed primary material into a dryer, and drying at 60° C. for 2 hours to obtain a dried material;(4)将上述得到的干燥料添加到双螺杆挤出机中进行熔融挤出造粒,得到色母粒;(4) adding the dry material obtained above into a twin-screw extruder to carry out melt extrusion granulation to obtain color masterbatch;其中,双螺杆挤出机的挤出温度为200℃。Wherein, the extrusion temperature of the twin-screw extruder is 200°C.
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