WO2020087550A1 - 一种纤维素/三聚氰胺甲醛复合树脂及其制备方法 - Google Patents
一种纤维素/三聚氰胺甲醛复合树脂及其制备方法 Download PDFInfo
- Publication number
- WO2020087550A1 WO2020087550A1 PCT/CN2018/113930 CN2018113930W WO2020087550A1 WO 2020087550 A1 WO2020087550 A1 WO 2020087550A1 CN 2018113930 W CN2018113930 W CN 2018113930W WO 2020087550 A1 WO2020087550 A1 WO 2020087550A1
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- WO
- WIPO (PCT)
- Prior art keywords
- cellulose
- melamine formaldehyde
- composite resin
- powder
- formaldehyde composite
- Prior art date
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Classifications
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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
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08L61/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08L61/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
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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
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/02—Cellulose; Modified cellulose
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/06—Polymer mixtures characterised by other features having improved processability or containing aids for moulding methods
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Definitions
- the present application relates to the technical field of polymer materials, in particular to a cellulose / melamine formaldehyde composite resin and a preparation method thereof.
- Melamine formaldehyde resin also known as melamine resin
- melamine resin is obtained by polycondensation of melamine and formaldehyde in a suitable medium.
- the resin is widely used in daily necessities such as porcelain tableware and electrical appliances.
- melamine formaldehyde resin has the disadvantages of high brittleness, poor toughness, and easy to crack under stress.
- Cellulose biomass powders such as plant stalks, crop straw powders, cereal husk powders, and cereal flours, are widely used in melamine formaldehyde resins.
- This melamine formaldehyde resin / cellulose powder composite material is manufactured by high-temperature molding.
- This melamine formaldehyde resin / cellulose powder molded product has poor strength and is more likely to fall apart than melamine resin. In order to increase strength, products are often made thick and heavy.
- Toughening modifiers are generally added during synthesis from the preparation of melamine resins.
- Chinese Patent No. 25, 2009 Publication No .: CN101585953A discloses a method for preparing melamine formaldehyde molding compound. Melamine and modifier are added to the kettle for reaction to obtain melamine formaldehyde molding compound.
- the modifier is polyvinyl alcohol, polyethylene glycol, p-toluene sulfonamide, dicyandiamide, and benzomelamine, any one or more of which can be mixed in any ratio. After modification, the strength and toughness of the molding compound are improved.
- Cipheral Patent November 16, 2016 discloses an amino molding compound powder used for processing melamine tableware and its preparation method. It consists of melamine resin molding compound, wood fiber, and sodium citrate , Titanium dioxide and zinc stearate.
- the melamine formaldehyde resin produced in the prior art still has various problems such as high brittleness, easy to drop, and the addition of biomass cellulose powder with poor composite strength and complex composition, the strength of the resulting melamine formaldehyde resin / cellulose powder molded product It can break easily when it is poor, stressed or dropped.
- this application proposes a cellulose / melamine formaldehyde composite resin and its preparation method, which has a good toughening effect, effectively improves the shortcomings of poor strength, easy to break when stressed or dropped, and the process is simple ,low cost.
- a cellulose / melamine formaldehyde composite resin proposed in this application its raw materials include, by weight percentage: melamine formaldehyde resin 30-90%, cellulose powder 5-60%, curing agent 0.01-0.1%, inorganic filler 0-20% , Surface modifier 1-5%, dimer acid 1-20%.
- the surface modifier is at least one of zinc stearate, calcium stearate, and silicon-anhui coupling agent.
- the cellulose powder is at least one of plant stalk powder, cereal powder, and cereal husk powder.
- This application uses plant stem powder, grain flour, grain hull powder, which is a natural renewable plant fiber, as a raw material for production. It is purely natural, non-polluting, and non-toxic. Plant stem powder, grain flour, and grain hull powder are discarded. In the past, the treatment of the crops was a problem. The long-term stacking caused the surrounding environment to be dirty and messy. The incineration process will bring serious air pollution, generate a large amount of carbon dioxide and sulfur dioxide, and will also bury the hidden danger of fire and even destroy the soil structure.
- Plant stalk powder, grain flour, and grain hull powder are renewable biopolymer materials with huge output on the earth.
- crop waste resources in addition to being safe and environmentally friendly, it is harmless to the human body and can replace traditional materials.
- plastic, melamine, etc. this natural renewable plant fiber is used as a raw material for production.
- This pays more attention to health and environmental protection concepts. It has no potential impact and harm on human bodies. This is an environmentally friendly high
- the efficient production method not only realizes the farmers' income generation again, brings objective and practical benefits to the farmers, but also protects the atmosphere and soil environment. More importantly, it avoids the problems of felling trees and chemical pollution in the production of traditional materials. After being discarded, it can be degraded in the natural environment, which reduces the environmental pollution in the process of agricultural waste disposal, and its degradability further eliminates white pollution.
- the inorganic filler is at least one of alumina, calcium carbonate, silica, and montmorillonite.
- the alumina, calcium carbonate, silica, and montmorillonite added in this application as inorganic fillers can weaken the strength of the product caused by the addition of a large amount of cellulose powder, and can increase the strength of the product.
- the preparation method of the cellulose / melamine formaldehyde composite resin proposed in this application is obtained by stirring the raw materials, sieving, and molding.
- the above raw materials are solid powders.
- the stirring time is 10-30 min, and the temperature during stirring is 40-60 ° C.
- the screen used for sieving is 80 mesh.
- the molding temperature is 140-180 ° C.
- the molding pressure is 500-2000 kN
- the molding time is 2-10 min.
- Dimer acid can react with melamine formaldehyde resin to introduce a flexible chain structure.
- the toughening effect is obvious, which can significantly improve the brittleness of melamine formaldehyde resin products.
- Dimer acid is used as a traditional chemical product at a price Low; Compared with the melamine formaldehyde resin in the prior art, the present application adds a toughening agent during the stirring process, and the process is simple.
- a cellulose / melamine formaldehyde composite resin its raw materials include: melamine formaldehyde resin 88.9kg, cellulose powder 5kg, curing agent 0.1kg, surface modifier 5kg, dimer acid 1kg.
- a cellulose / melamine formaldehyde composite resin its raw materials include: melamine formaldehyde resin 30.99kg, cellulose powder 8kg, curing agent 0.01kg, inorganic filler 10kg, surface modifier 1kg, dimer acid 10kg.
- a cellulose / melamine formaldehyde composite resin the raw materials of which include: melamine formaldehyde resin 30kg, plant stem 28.98kg, curing agent 0.02kg, montmorillonite 20kg, zinc stearate 1kg, dimer acid 20kg.
- a cellulose / melamine formaldehyde composite resin its raw materials include: melamine formaldehyde resin 45kg, cellulose powder 32.94kg, curing agent 0.06kg, inorganic filler 12kg, surface modifier 5kg, dimer acid 5kg.
- the cellulose powder is cereal powder and cereal skin powder.
- the inorganic filler is alumina and montmorillonite.
- the surface modifier is zinc stearate and silicon-anhui coupling agent.
- the preparation method of the above cellulose / melamine formaldehyde composite resin includes the following steps: the above raw materials are stirred for 10 minutes, the temperature during the stirring is 60 ° C., passed through an 80 mesh sieve, and molded at 140 ° C. for 10 minutes, and the molding pressure is 500-kN. .
- a cellulose / melamine formaldehyde composite resin its raw materials include: melamine formaldehyde resin 35.97kg, cellulose powder 60kg, curing agent 0.03kg, inorganic filler 1kg, surface modifier 1kg, dimer acid 2kg.
- Cellulose powder includes plant stalk powder, grain powder, and grain hull powder.
- Inorganic fillers include alumina, calcium carbonate, silica, and montmorillonite.
- Surface modifiers include zinc stearate, calcium stearate, and silicon-anhui coupling agent.
- the preparation method of the above cellulose / melamine formaldehyde composite resin includes the following steps: the above raw materials are stirred for 30 minutes, the temperature during the stirring is 40 ° C., passed through an 80-mesh sieve, and molded at 180 ° C. for 2 minutes, and the molding pressure is 1980 kN.
- a cellulose / melamine formaldehyde composite resin the raw materials of which include: melamine formaldehyde resin 40kg, rice husk powder 50kg, curing agent 0.1kg, alumina 5kg, zinc stearate 2kg, dimer acid 3kg.
- the preparation method of the above cellulose / melamine formaldehyde composite resin includes the following steps: the above raw materials are stirred for 10 minutes, the temperature during the stirring is 60 ° C, passed through an 80-mesh sieve, and molded at 150 ° C for 5 minutes, and the molding pressure is 2000 kN.
- a cellulose / melamine formaldehyde composite resin its raw materials include: melamine formaldehyde resin 40kg, rice husk powder 50kg, curing agent 0.1kg, alumina 5kg, zinc stearate 2kg.
- the preparation method of the above cellulose / melamine formaldehyde composite resin includes the following steps: stirring the above raw materials for 10 minutes, the temperature during the stirring is 60 ° C., passing through an 80-mesh sieve, molding at 150 ° C. for 5 min, and molding pressure at 2000 kN.
- a cellulose / melamine formaldehyde composite resin its raw materials include: melamine formaldehyde resin 40kg, bamboo fiber powder 40kg, curing agent 0.1kg, calcium stearate 5kg, dimer acid 15kg.
- the preparation method of the above cellulose / melamine formaldehyde composite resin includes the following steps: the above raw materials are stirred for 20 minutes, the temperature during the stirring is 50 ° C., passed through an 80-mesh sieve, molded at 150 ° C. for 5 minutes, and the molded pressure is 2000 kN.
- a cellulose / melamine formaldehyde composite resin its raw materials include: melamine formaldehyde resin 40kg, bamboo fiber powder 40kg, curing agent 0.1kg, calcium stearate 5kg.
- the preparation method of the above cellulose / melamine formaldehyde composite resin includes the following steps: the above raw materials are stirred for 20 minutes, the temperature during the stirring is 50 ° C., passed through an 80-mesh sieve, and molded at 150 ° C. for 5 minutes, and the molding pressure is 2000 kN.
- a cellulose / melamine formaldehyde composite resin its raw materials include: melamine formaldehyde resin 30kg, rice straw powder 50kg, curing agent 0.1kg, 300 mesh silica powder 10kg, silane coupling agent KH-550 2kg, calcium stearate 3kg, 5kg dimer acid.
- the preparation method of the above cellulose / melamine formaldehyde composite resin includes the following steps: the above raw materials are stirred for 20 minutes, the temperature during the stirring is 50 ° C., passed through an 80-mesh sieve, and molded at 160 ° C. for 2 minutes, and the molding pressure is 2000 kN.
- a cellulose / melamine formaldehyde composite resin its raw materials include: melamine formaldehyde resin 30kg, rice straw powder 50kg, curing agent 0.1kg, 300 mesh silica powder 10kg, silane coupling agent KH-550 2kg, calcium stearate 3kg.
- the preparation method of the above cellulose / melamine formaldehyde composite resin includes the following steps: the above raw materials are stirred for 20 minutes, the temperature during the stirring is 50 ° C., passed through an 80-mesh sieve, and molded at 160 ° C. for 2 minutes, and the molding pressure is 2000 kN.
- a cellulose / melamine formaldehyde composite resin its raw materials include: melamine formaldehyde resin 40kg, corn starch 50kg, curing agent 0.1kg, calcium stearate 5kg, dimer acid 5kg.
- the preparation method of the above cellulose / melamine formaldehyde composite resin includes the following steps: the above raw materials are stirred for 20 minutes, the temperature during the stirring is 50 ° C., passed through an 80-mesh sieve, and molded at 160 ° C. for 2 min.
- the molding pressure is 2000 kN.
- a cellulose / melamine formaldehyde composite resin its raw materials include: melamine formaldehyde resin 40kg, corn starch 40kg, curing agent 0.1kg, calcium stearate 5kg.
- the preparation method of the above cellulose / melamine formaldehyde composite resin includes the following steps: the above raw materials are stirred for 20 minutes, the temperature during the stirring is 50 ° C, passed through an 80-mesh sieve, and molded at 160 ° C for 2 minutes, and the molding pressure is 2000 kN.
- the cellulose / melamine formaldehyde composite resin obtained in Example 6-9 and the cellulose / melamine formaldehyde composite resin obtained in Comparative Example were respectively made into samples with a size of 5 cm ⁇ 20 cm ⁇ 0.5 cm, and the samples were subjected to a drop test as follows : Place the sample parallel to the ground at a height of 2m, and then let it fall freely. Test 50 times in parallel for each group of samples. Count the damage (cracks or breaks) after the drop. The results are as follows:
- this application introduces a flexible chain structure through the reaction of dimer acid and melamine formaldehyde resin, which has obvious toughening effect and can significantly improve the brittleness of melamine formaldehyde resin products.
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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)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
测试项目 | 测试结果 |
实施例6 | 1% |
对比例1 | 35% |
实施例7 | 2% |
对比例2 | 38% |
实施例8 | 4% |
对比例3 | 46% |
实施例9 | 1% |
对比例4 | 32% |
Claims (8)
- 一种纤维素/三聚氰胺甲醛复合树脂,其特征在于,其原料按重量百分比包括:三聚氰胺甲醛树脂30-90%,纤维素粉5-60%,固化剂0.01-0.1%,无机填料0-20%,表面改性剂1-5%,二聚酸1-20%。
- 根据权利要求1所述纤维素/三聚氰胺甲醛复合树脂,其特征在于,纤维素粉为植物茎秆粉、谷粉、谷类皮壳粉中至少一种。
- 根据权利要求1-2任一项所述纤维素/三聚氰胺甲醛复合树脂,其特征在于,无机填料为氧化铝、碳酸钙、二氧化硅、蒙脱土中至少一种。
- 根据权利要求1-3任一项所述纤维素/三聚氰胺甲醛复合树脂,其特征在于,表面改性剂为硬脂酸锌、硬脂酸钙、硅皖偶联剂中至少一种。
- 一种如权利要求1-4任一项所述纤维素/三聚氰胺甲醛复合树脂制备方法,其特征在于,包括如下步骤:将原料进行搅拌,过筛,模压成型即得。
- 根据权利要求5所述纤维素/三聚氰胺甲醛复合树脂制备方法,其特征在于,搅拌时间为10-30min,搅拌过程中温度为40-60℃。
- 根据权利要求5或6所述纤维素/三聚氰胺甲醛复合树脂制备方法,其特征在于,过筛所用筛网为80目。
- 根据权利要求5-7任一项所述纤维素/三聚氰胺甲醛复合树脂制备方法,其特征在于,模压成型温度为140-180℃,模压成型压力为500-2000kN,模压成型时间为2-10min。
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US16/307,149 US11053383B1 (en) | 2018-10-31 | 2018-11-05 | Cellulose/melamine-formaldehyde composite resin and preparation method thereof |
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CN201811285171.8A CN109504031A (zh) | 2018-10-31 | 2018-10-31 | 一种纤维素/三聚氰胺甲醛复合树脂及其制备方法 |
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CN113004653A (zh) * | 2021-04-25 | 2021-06-22 | 晋江市旭佰日用品有限责任公司 | 一种环保无毒密胺树脂餐具及其制备方法 |
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CN115466484A (zh) * | 2022-03-16 | 2022-12-13 | 深圳市德艺科技实业有限公司 | 一种含天然纤维的密胺树脂制品及其制备方法 |
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