CN111333995A - High-temperature-resistant and high-strength ammonia-free phenolic moulding plastic and preparation method thereof - Google Patents
High-temperature-resistant and high-strength ammonia-free phenolic moulding plastic and preparation method thereof Download PDFInfo
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- CN111333995A CN111333995A CN202010334959.4A CN202010334959A CN111333995A CN 111333995 A CN111333995 A CN 111333995A CN 202010334959 A CN202010334959 A CN 202010334959A CN 111333995 A CN111333995 A CN 111333995A
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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
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a high-temperature-resistant and high-strength ammonia-free phenolic molding compound and a preparation method thereof, and relates to the technical field of special engineering plastics. The technical key points are as follows: a high-temperature-resistant and high-strength ammonia-free phenolic molding compound comprises the following components in parts by weight: 60-100 parts of phenolic resin; 10-30 parts of melamine formaldehyde resin; 5-10 parts of urea-formaldehyde resin; 1-5 parts of calcium oxide; 20-40 parts of inorganic filler; 40-80 parts of reinforcing fiber; 1-5 parts of a lubricant; the invention also discloses a preparation method of the high-temperature-resistant and high-strength ammonia-free phenolic moulding plastic, which comprises the following steps: putting the phenolic resin, the melamine formaldehyde resin, the urea formaldehyde resin, the calcium oxide, the inorganic filler, the reinforcing fiber and the lubricant in corresponding parts by weight into an open type plastic refining machine for mixing, wherein the temperature of an operation roller of the open type plastic refining machine is 90-110 ℃, the temperature of a heating roller is 140-150 ℃, the distance between rollers is 3-4mm, and the mixing time is 5-6 mim. The phenolic moulding plastic prepared by the invention has the advantages of high temperature resistance, high strength and no ammonia residue.
Description
Technical Field
The invention relates to the technical field of special engineering plastics, in particular to a high-temperature-resistant high-strength ammonia-free phenolic molding compound and a preparation method thereof.
Background
A powdered phenolic moulding material is prepared from phenolic resin as adhesive, wood powder as filler and additive through hot smelting. It is suitable for compression molding and injection molding, and can be used for low-voltage electrical appliances, common household appliances, flame-retardant, heat-resistant and water-resistant high-strength electrical appliance accessories, water-lubricated bearings and sealing rings, high-performance automobile parts, insulating structural parts of traffic electrical appliances, telecommunication and radio insulating parts with high-frequency insulativity and the like.
The Chinese patent with publication number CN107141709B discloses a composite modified phenolic molding compound for motors, which comprises 600 parts of 300-50 parts of phenolic resin, 10-50 parts of dicyclopentadiene epoxy resin, 600 parts of 400-600 parts of inorganic fiber, 250 parts of nano inorganic filler, 10-50 parts of release agent, 50-100 parts of curing agent, 10-30 parts of low-temperature accelerant and 10-100 parts of high-temperature accelerant.
The composite modified phenolic molding compound for the motor has the characteristics of high mechanical strength, high cohesiveness, low molding shrinkage and high dimensional stability, and shows excellent performance of cracking of a finished product in the aspect of application. However, the curing agents used in the method can be trimethylolmelamine, triethylamine and hexamethylenetetramine, so that the produced phenolic molding compound can generate ammonia gas volatilization in a downstream production process.
Therefore, a new solution is needed to solve the above problems.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a high-temperature-resistant and high-strength ammonia-free phenolic molding compound which has the advantages of high temperature resistance, high strength and no ammonia residue.
The second purpose of the invention is to provide a preparation method of the high-temperature-resistant and high-strength ammonia-free phenolic moulding plastic, which has the advantages of simple operation and suitability for large-scale production.
In order to achieve the first purpose, the invention provides the following technical scheme:
a high-temperature-resistant and high-strength ammonia-free phenolic molding compound comprises the following components in parts by weight:
phenolic resin: 60-100 parts;
melamine formaldehyde resin: 10-30 parts;
urea-formaldehyde resin: 5-10 parts;
calcium oxide: 1-5 parts;
inorganic filler: 20-40 parts;
reinforcing fibers: 40-80 parts;
lubricant: 1-5 parts.
By adopting the technical scheme, the phenolic molding compound obtained by using the phenolic resin as the adhesive, the melamine formaldehyde resin and the urea formaldehyde resin as the curing agents instead of the trimethylol melamine, the triethylamine and the hexamethylene tetramine and the calcium oxide as the curing accelerator has no free ammonia residue, the cost is reduced, the environment is friendly, and the product stability is good. The invention also adds inorganic filler and reinforced fiber into the raw material components, which can greatly improve the mechanical property of the phenolic moulding plastic and is suitable for low-voltage electrical appliances, common living appliances, high-strength electrical appliance accessories and the like.
More preferably, the phenol resin is a linear resin and/or a water-soluble phenol resin.
More preferably, 1-5 parts by weight of modified graphene is also added.
By adopting the technical scheme, the graphene is added into the raw material components instead of common wood powder, is a novel flaky material consisting of carbon atoms, and has excellent heat resistance and mechanical properties. Graphene can be compounded with phenolic resin, so that mechanical properties reduced by removing wood flour are supplemented and greatly improved.
More preferably, the modifying step of the modified graphene is: dissolving graphene in chloroform, adding tannic acid, adjusting the pH to be alkaline under the stirring condition, reacting for 12h, and removing the chloroform to obtain the graphene.
By adopting the technical scheme, strong intermolecular force exists among the graphene nano-sheets, so that the graphene sheets are easy to agglomerate and difficult to disperse in resin, and the toughening and reinforcing effects of the graphene filler on the resin can be greatly reduced. According to the invention, the surface of the graphene is modified, so that the interface bonding effect between the graphene and the phenolic resin is improved, and the dispersion stability of the graphene in the phenolic resin is improved.
Further preferably, the inorganic filler is selected from one or more of ground calcium carbonate, talc and wollastonite.
By adopting the technical scheme, the filler mainly plays a role in enhancing the mechanical strength of the phenolic moulding plastic and reducing the cost.
Further preferably, the reinforcing fibers are selected from one or more of glass fibers, basalt fibers and steel fibers.
By adopting the technical scheme, the phenolic resin can be more firmly reinforced by using the reinforced fiber, and the dimensional stability and the strength of the resin belt pulley can be further improved.
Further preferably, the lubricant is one or more selected from zinc stearate, ethylene bis stearamide, and fluororesin powder.
By adopting the technical scheme, the lubricant has better internal lubrication effect, so that the fluidity and the mold release property of the molten plastic are improved in the plastic molding processing, the yield of the plastic processing is improved, the energy consumption is reduced, and the product has extremely high surface smoothness and smoothness.
In order to achieve the second purpose, the invention provides the following technical scheme:
a preparation method of a high-temperature-resistant and high-strength ammonia-free phenolic molding compound comprises the following steps:
putting the phenolic resin, the melamine formaldehyde resin, the urea formaldehyde resin, the calcium oxide, the inorganic filler, the reinforcing fiber and the lubricant in corresponding parts by weight into an open type plastic refining machine for mixing, wherein the temperature of an operation roller of the open type plastic refining machine is 90-110 ℃, the temperature of a heating roller is 140-150 ℃, the distance between rollers is 3-4mm, and the mixing time is 5-6 mim.
By adopting the technical scheme, the preparation method can be used for mixing the multi-component raw materials at one time, has high production efficiency and is suitable for large-scale production.
In summary, compared with the prior art, the invention has the following beneficial effects:
(1) the phenolic molding compound has the advantages that the phenolic resin is used as the adhesive, melamine formaldehyde resin and urea formaldehyde resin are used for replacing trimethylol melamine, triethylamine and hexamethylene tetramine to be used as the curing agent, and calcium oxide is used as the curing accelerator, so that the obtained phenolic molding compound has no free ammonia residue, the cost is reduced, the environment is protected, and the product stability is good. The invention also adds inorganic filler and reinforced fiber into the raw material components, which can greatly improve the mechanical property of the phenolic moulding plastic and is suitable for low-voltage electrical appliances, common living appliances, high-strength electrical appliance accessories and the like;
(2) according to the invention, the graphene is added into the raw material components instead of common wood powder, and is a novel flaky material consisting of carbon atoms, so that the graphene has excellent heat resistance and mechanical properties. Graphene can be compounded with phenolic resin, so that the mechanical property reduced by removing wood powder is supplemented and greatly improved;
(3) according to the invention, the surface of the graphene is modified, so that the interface bonding effect between the graphene and the phenolic resin is improved, and the dispersion stability of the graphene in the phenolic resin is improved.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1: the high-temperature-resistant and high-strength ammonia-free phenolic molding plastic is prepared by the following steps of:
according to the table 1, the phenolic resin, the melamine formaldehyde resin, the urea formaldehyde resin, the calcium oxide, the inorganic filler, the reinforcing fiber and the lubricant in corresponding parts by weight are put into an open type plastic mixer for mixing, wherein the operating roller temperature of the open type plastic mixer is 90 ℃, the heating roller temperature is 140 ℃, the roller interval is 3mm, and the mixing time is 5 mim.
The phenolic resin in the embodiment adopts linear bisphenol A phenolic resin with the molecular weight of 2000 and the hydroxyl equivalent of 150; the inorganic filler adopts heavy calcium carbonate; the reinforcing fiber is glass fiber; the lubricant is calcium stearate.
Examples 2 to 6: a high-temperature-resistant and high-strength ammonia-free phenolic molding compound is different from the compound in example 1 in that the components and the corresponding parts by weight are shown in Table 1.
TABLE 1 Components and parts by weight of examples 1-6
Example 7: a high-temperature-resistant and high-strength ammonia-free phenolic molding compound is different from the compound prepared in the example 1 in that the compound is prepared by the following steps:
according to the table 1, the phenolic resin, the melamine formaldehyde resin, the urea formaldehyde resin, the calcium oxide, the inorganic filler, the reinforcing fiber and the lubricant were put into an open type plasticator and mixed, the operating roll temperature of the open type plasticator was 110 ℃, the heating roll temperature was 150 ℃, the roll interval was 4mm, and the mixing time was 6 mm.
In this embodiment, the phenolic resin is a water-soluble phenolic resin selected from Dahua brand produced by Wuhan Dahuawei pharmaceutical chemical Co.
Example 8: a high-temperature-resistant and high-strength ammonia-free phenolic molding compound is different from the compound in the embodiment 1 in that the inorganic filler is a mixture of heavy calcium carbonate and talcum powder in a weight ratio of 1: 1.
Example 9: the difference between the high-temperature-resistant and high-strength ammonia-free phenolic molding compound and the phenolic molding compound in the example 1 is that the inorganic filler is a mixture of ground limestone, talcum powder and wollastonite in a weight ratio of 1:1: 0.2.
Example 10: the difference between the high-temperature-resistant and high-strength ammonia-free phenolic molding compound and the phenolic molding compound in the embodiment 1 is that the reinforcing fiber is a mixture of glass fiber and basalt fiber in a weight ratio of 1: 0.6.
Example 11: the difference between the high-temperature-resistant and high-strength ammonia-free phenolic molding compound and the phenolic molding compound in the embodiment 1 is that the reinforcing fibers are a mixture of glass fibers, basalt fibers and steel fibers in a weight ratio of 1:0.6: 0.5.
Example 12: a high temperature resistant, high strength ammonia free phenolic moulding compound, which differs from example 1 in that the lubricant is a mixture of zinc stearate and ethylene bis stearamide in a weight ratio of 1: 1.
Example 13: a high temperature resistant, high strength ammonia free phenolic moulding compound, which differs from example 1 in that the lubricant is a mixture of zinc stearate, ethylene bis stearamide and fluororesin powder in a weight ratio of 1:1: 1.
Example 14: the difference between the high-temperature-resistant and high-strength ammonia-free phenolic moulding plastic and the embodiment 1 is that 1 part by weight of modified graphene is added when raw material components are mixed again.
The preparation method of the modified graphene in this embodiment is as follows:
adding 40g of graphite X into 1.5L of chloroform, adding 130g of tannic acid, dropwise adding strong sodium oxide until the pH value is 10, stirring and reacting for 12 hours, and after the reaction is finished, carrying out rotary evaporation at 38 ℃ to remove chloroform, thus obtaining the modified graphene.
Comparative example 1: a phenolic molding material, different from example 1 in that wood flour is used to replace melamine formaldehyde resin and urea formaldehyde resin, the fineness of the wood flour in the comparative example is 120 meshes, the water content is less than or equal to 8%, and the apparent density is 0.2mg/cm3。
Comparative example 2: a phenolic molding compound which differs from example 1 in that no melamine formaldehyde resin and no urea formaldehyde resin are added.
Comparative example 3: a phenolic moulding compound differs from example 1 in that no calcium oxide is added.
Comparative example 4: a phenolic molding compound, which is different from the phenolic molding compound in example 1 in that graphene is not modified.
Performance testing
The phenolic molding materials prepared in examples 1 to 14 and comparative examples 1 to 4 were subjected to performance tests, and the test results are shown in Table 2 below.
As can be seen from the test data in Table 2, the heat distortion temperature of examples 1 to 14 under a load of 1.8MPa reached 275 ℃ or higher, the flexural strength reached 275MPa or higher, and the notched impact strength reached 3.1/KJ · m-2Above that, the unnotched impact strength reaches 7.1/KJ.m-2The above. In the embodiment 14, as the homemade modified graphene is added, the thermal deformation temperature reaches 295 ℃, the mechanical properties are higher than those of other embodiments, and the best embodiment is shown in the comparative example 1, wood flour is used for replacing melamine formaldehyde resin and urea formaldehyde resin, the thermal deformation temperature is 254 ℃, and the bending strength is 68.2 MPa; comparative example 2 the worst comparative example, in which the heat distortion temperature was 205 ℃ and the flexural strength was 62.8MPa, was obtained without adding the amine-formaldehyde resin and the urea-formaldehyde resin; comparative example 3 the thermal deformation temperature was 221 ℃ and the bending strength was 64.1MPa since calcium oxide was not added; the graphene added in comparative example 4 was not modified, and had a heat distortion temperature of 260 ℃ and a flexural strength of 74.2 MPa. In conclusion, the phenolic molding compound prepared by the invention has the advantages of high temperature resistance, high strength and no ammonia residue.
Table 2 results of performance testing
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.
Claims (8)
1. The high-temperature-resistant and high-strength ammonia-free phenolic molding compound is characterized by comprising the following components in parts by weight:
phenolic resin: 60-100 parts;
melamine formaldehyde resin: 10-30 parts;
urea-formaldehyde resin: 5-10 parts;
calcium oxide: 1-5 parts;
inorganic filler: 20-40 parts;
reinforcing fibers: 40-80 parts;
lubricant: 1-5 parts.
2. The high temperature resistant, high strength ammonia-free phenolic molding compound as claimed in claim 1, wherein the phenolic resin is a linear resin and/or a water soluble phenolic resin.
3. The high temperature resistant, high strength ammonia-free phenolic molding compound as claimed in claim 1, wherein 1-5 parts by weight of modified graphene is further added.
4. The high temperature resistant, high strength ammonia-free phenolic molding compound as claimed in claim 3, wherein the modification step of the modified graphene is as follows: dissolving graphene in chloroform, adding tannic acid, adjusting the pH to be alkaline under the stirring condition, reacting for 12h, and removing the chloroform to obtain the graphene.
5. The high temperature resistant, high strength, ammonia free phenolic molding compound of claim 1, wherein the inorganic filler is selected from one or more of ground calcium carbonate, talc and wollastonite.
6. The high temperature resistant, high strength ammonia free phenolic molding compound of claim 1, wherein said reinforcing fibers are selected from one or more of the group consisting of glass fibers, basalt fibers, and steel fibers.
7. The high temperature resistant, high strength ammonia free phenolic molding compound as claimed in claim 1, wherein said lubricant is selected from one or more of zinc stearate, ethylene bis stearamide and fluororesin powder.
8. The method for preparing a high temperature resistant, high strength ammonia free phenolic molding compound as claimed in any one of claims 1 to 7, comprising the steps of:
putting the phenolic resin, the melamine formaldehyde resin, the urea formaldehyde resin, the calcium oxide, the inorganic filler, the reinforcing fiber and the lubricant in corresponding parts by weight into an open type plastic refining machine for mixing, wherein the temperature of an operation roller of the open type plastic refining machine is 90-110 ℃, the temperature of a heating roller is 140-150 ℃, the distance between rollers is 3-4mm, and the mixing time is 5-6 mim.
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| CN202010334959.4A CN111333995A (en) | 2020-04-24 | 2020-04-24 | High-temperature-resistant and high-strength ammonia-free phenolic moulding plastic and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112708241A (en) * | 2020-12-29 | 2021-04-27 | 江苏森博新材料有限公司 | Ammonia-free phenolic moulding plastic and its production method |
| CN114933775A (en) * | 2022-05-26 | 2022-08-23 | 浙江嘉民新材料有限公司 | Heat-resistant high-strength ammonia-free phenolic aldehyde injection molding material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1958662A (en) * | 2006-10-30 | 2007-05-09 | 林良菽 | Plastic of phenolic aldehyde mould in no ammonia type, and manufacturing method |
| CN105385100A (en) * | 2015-12-23 | 2016-03-09 | 江南大学 | Graphene-modified phenolic molding material and preparation method thereof |
| CN109517331A (en) * | 2018-11-30 | 2019-03-26 | 江苏中鹏新材料股份有限公司 | Without ammonia high intensity phenolaldehyde moulding compound and preparation method thereof |
-
2020
- 2020-04-24 CN CN202010334959.4A patent/CN111333995A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1958662A (en) * | 2006-10-30 | 2007-05-09 | 林良菽 | Plastic of phenolic aldehyde mould in no ammonia type, and manufacturing method |
| CN105385100A (en) * | 2015-12-23 | 2016-03-09 | 江南大学 | Graphene-modified phenolic molding material and preparation method thereof |
| CN109517331A (en) * | 2018-11-30 | 2019-03-26 | 江苏中鹏新材料股份有限公司 | Without ammonia high intensity phenolaldehyde moulding compound and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112708241A (en) * | 2020-12-29 | 2021-04-27 | 江苏森博新材料有限公司 | Ammonia-free phenolic moulding plastic and its production method |
| CN114933775A (en) * | 2022-05-26 | 2022-08-23 | 浙江嘉民新材料有限公司 | Heat-resistant high-strength ammonia-free phenolic aldehyde injection molding material |
| CN114933775B (en) * | 2022-05-26 | 2023-06-20 | 浙江嘉民新材料有限公司 | Heat-resistant high-strength ammonia-free phenolic injection molding material |
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