CN105647103A - Modified polyformaldehyde composite material and preparation method thereof - Google Patents
Modified polyformaldehyde composite material and preparation method thereof Download PDFInfo
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- CN105647103A CN105647103A CN201410627502.7A CN201410627502A CN105647103A CN 105647103 A CN105647103 A CN 105647103A CN 201410627502 A CN201410627502 A CN 201410627502A CN 105647103 A CN105647103 A CN 105647103A
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Abstract
The invention discloses a modified polyformaldehyde composite material. The modified polyformaldehyde composite material is prepared from the following raw materials in parts by weight: 80-95 parts of polyformaldehyde, 5-20 parts of pretreated molybdenum disulfide, 0.1-2.0 parts of thermal stabilizer and 0.5-1.0 part of lubricant. The invention further discloses a preparation method for the modified polyformaldehyde composite material. The preparation method comprises the steps: (1) proportionally weighing the raw materials, adding the weighed raw materials into a high-speed mixer, and carrying out mixing for 2 to 10 minutes; (2) subjecting the mixture obtained in the step (1) to extruded granulating in a co-rotating parallel twin-screw extruder at the temperature of 150 DEG C to 180 DEG C; and (3) subjecting granules obtained in the step (2) to injection molding in an equidirectional twin-screw injection molding machine at the temperature of 150 DEG C to 180 DEG C. The polyformaldehyde composite material prepared by the preparation method has the excellent properties of wear resistance and lubrication, thereby being capable of being extensively applied to the field of plastic modification.
Description
Technical field
The present invention relates to polymeric material field, particularly relate to a kind of improved polyoxymethylene composite and preparation technology thereof.
Background technology
Polyoxymethylene is the engineering plastics of a kind of high comprehensive performance, there are extremely high strength and stiffness, good dimensional stability, excellent resistance to fatigue, creep resistant, self lubricity and wear resisting property, extensively for the manufacture of the various part with low frictional coefficient wearable performance in machinery, automobile, electronics, household electrical appliances and building materials etc. But polyoxymethylene poor heat stability at high temperature, easily decompose; And its machine-shaping temperature is narrow, and ageing resistance is poor, only can use when low speed, underload. In order to make polyoxymethylene use under the severe condition such as high speed, high loading, just on the basis of the physical and mechanical properties of original excellence, must reducing its frictional coefficient and wear rate further, with regard to needing, the modification by polyoxymethylene realizes for this.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes the deficiency of existing polyformaldehyde material, it is provided that a kind of low frictional coefficient wearable, preparation technology are simple, cost is lower improved polyoxymethylene composite and its preparation method.
The present invention solves the technical scheme that told technical problem adopts:
A kind of improved polyoxymethylene composite, it is made up by weight of following raw material:
Polyoxymethylene 80-95 part
Pretreated molybdenumdisulphide 5-20 part
Thermo-stabilizer 0.1��2.0 part
Lubricant 0.5-1.0 part
Described pretreated molybdenumdisulphide adopts following step method to obtain:
(1) molybdenumdisulphide of 1-10kg is joined in the dilution heat of sulfuric acid of 15wt%-20wt% of 5-10L, it is heated to 50-80 DEG C, stir 1-2 hour, filter, with deionized water wash to neutral; It is the sodium hydroxide solution of 15wt%-20wt% that molybdenumdisulphide after trace impurity is removed in washing joins the concentration of 5-10L, 50-80 DEG C, stirs 1-2 hour, filters, with deionized water wash to neutral, dry;
(2) dried molybdenumdisulphide is added in the ethanolic soln of titanate coupling agent of 5-10L, infiltrate 30-60 minute, filter, dry, obtain pretreated molybdenumdisulphide; The ethanol solution concentration of described titanate coupling agent is 0.1wt%-1wt%.
Wherein, the object of described step (1) is: 1, remove molybdenumdisulphide surface impurity; 2, slight erosion molybdenumdisulphide surface, increases the roughness on molybdenumdisulphide surface, it is to increase the consistency of polymkeric substance and mechanical property. Dilute sulphuric acid and concentration of sodium hydroxide solution, Heating temperature is too high or churning time is too long even can dissolve molybdenumdisulphide by heavy corrosion molybdenumdisulphide, greatly destroys the performance of molybdenumdisulphide itself; Concentration, Heating temperature are too low, churning time is short, do not have the due effect of this step.
Step (2) described titanate coupling agent can be titanate coupling agent UP-131.
Described molybdenumdisulphide purity >=98%, median size 10nm, specific surface area 200m2/g. Here particle diameter and specific surface area can not be too little, and too little meeting causes reunion serious between powder body; Can not be too big, too big particle diameter can make compatibility poor. The diamond of this particle diameter and specific surface area is after acid-alkali treatment, and degree of being corroded is also relatively good, after coupling agent treatment, and the wear resistance of the raising composition of energy maximum amplitude and other mechanical properties.
Further, the melting index of described polyoxymethylene is 9g/10min.
Further, described thermo-stabilizer is at least one in trimeric cyanamide, polymeric amide, Hinered phenols antioxidant. Wherein Hinered phenols antioxidant comprises antioxidant 1010 (four [methyl-��-(3,5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester), irgasfos 168 (three �� 2.4-di-tert-butyl-phenyl �� phosphorous acid ester).
Further, described lubricant is at least one of white oil, silicone oil, paraffin, stearic acid, calcium stearate, Zinic stearas.
Another technical scheme of the present invention is to provide the preparation method of above-mentioned improved polyoxymethylene composite, comprises the following steps:
(1) raw material is weighed in proportion join in high-speed mixer, mixing 2-10min;
(2) by step (1) gained mixture at equidirectional parallel double-screw extruder extruding pelletization, temperature is 150-180 DEG C;
(3) by the injection moulding in parallel dual-screw injection moulding machine of step (2) gained pellet, temperature is 150-180 DEG C.
The polyformaldehyde composite material that the present invention obtains has excellent properties wear-resisting, lubrication, can be used in modifying plastics field widely.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
Molybdenumdisulphide pre-treatment step is as follows:
(1) molybdenumdisulphide of 1kg is joined in the dilution heat of sulfuric acid of 15wt% of 5L, it is heated to 50 DEG C, stir 1 hour, filter, with deionized water wash to neutral; Concentration molybdenumdisulphide after removal trace impurity being joined 5L is the sodium hydroxide solution of 15wt%, 50 DEG C, stirs 1 hour, filters, with deionized water wash to neutral, dry;
(2) concentration that pretreated molybdenumdisulphide adds 5L is in the ethanolic soln of titanate coupling agent UP-131 of 0.1wt%, infiltrates 30 minutes, filters, and dries, obtains pretreated molybdenumdisulphide.
The preparation process of improved polyoxymethylene composite is as follows:
Raw material weight proportioning is: polyoxymethylene 90 parts, pretreated molybdenumdisulphide 10 parts, antioxidant 1010 1 part, irgasfos 168 1 part, silicone oil 0.5 part, calcium stearate 0.5 part.
(1) above-mentioned raw materials is weighed in proportion join in high-speed mixer, mixing 5min;
(2) by step (1) gained mixture at equidirectional parallel double-screw extruder extruding pelletization, temperature is 150 DEG C, a district, two 170 DEG C, districts, three 180 DEG C, districts, four 180 DEG C, districts, five 180 DEG C, districts;
(3) by the injection moulding in parallel dual-screw injection moulding machine of step (2) gained pellet, temperature is 150 DEG C, a district, two 170 DEG C, districts, three 180 DEG C, districts, four 180 DEG C, districts, five 180 DEG C, districts. The present embodiment products obtained therefrom performance test methods standard number and test result arrange in table 1.
Embodiment 2
Molybdenumdisulphide pre-treatment step is as follows:
(1) molybdenumdisulphide of 2kg is joined in the dilution heat of sulfuric acid of 18wt% of 6L, it is heated to 60 DEG C, stir 1.5 hours, filter, with deionized water wash to neutral; Concentration molybdenumdisulphide after removal trace impurity being joined 8L is the sodium hydroxide solution of 18wt%, 60 DEG C, stirs 1.5 hours, filters, with deionized water wash to neutral, dry;
(2) concentration that pretreated molybdenumdisulphide adds 8L is in monoalkoxy lipid acid titanate coupling agent (titanate coupling agent UP-131) ethanolic soln of 0.5wt%, infiltrates 40 minutes, filters, and dries, obtains pretreated molybdenumdisulphide.
The preparation process of improved polyoxymethylene composite is as follows:
The present embodiment raw material weight proportioning is: polyoxymethylene 85 parts, pretreated molybdenumdisulphide 15 parts, antioxidant 1010 0.1 part, silicone oil 0.5 part.
Preparation method:
(1) raw material is weighed in proportion join in high-speed mixer, mixing 2min;
(2) by step (1) gained mixture at equidirectional parallel double-screw extruder extruding pelletization, temperature is 150 DEG C, a district, two 170 DEG C, districts, three 180 DEG C, districts, four 180 DEG C, districts, five 180 DEG C, districts;
(3) by the injection moulding in parallel dual-screw injection moulding machine of step (2) gained pellet, temperature is 150 DEG C, a district, two 170 DEG C, districts, three 180 DEG C, districts, four 180 DEG C, districts, five 180 DEG C, districts.
The present embodiment product test the results are shown in table 1.
Embodiment 3
Molybdenumdisulphide pre-treatment step is as follows:
(1) molybdenumdisulphide of 10kg is joined in the dilution heat of sulfuric acid of 20wt% of 10L, it is heated to 80 DEG C, stir 2 hours, filter, with deionized water wash to neutral; Concentration molybdenumdisulphide after removal trace impurity being joined 10L is the sodium hydroxide solution of 20wt%, 80 DEG C, stirs 2 hours, filters, with deionized water wash to neutral, dry;
(2) concentration that pretreated molybdenumdisulphide adds 10L is in monoalkoxy lipid acid titanate coupling agent (titanate coupling agent UP-131) ethanolic soln of 1wt%, infiltrates 60 minutes, filters, and dries, obtains pretreated molybdenumdisulphide.
The preparation process of improved polyoxymethylene composite is as follows:
Raw material weight proportioning is: polyoxymethylene 80 parts, pretreated molybdenumdisulphide 20 parts, antioxidant 1010 1 part, irgasfos 168 0.5 part, white oil 0.5 part, 0.5 part, paraffin.
Preparation method:
(1) raw material is weighed in proportion join in high-speed mixer, mixing 8min;
(2) by step (1) gained mixture at equidirectional parallel double-screw extruder extruding pelletization, temperature is 150 DEG C, a district, two 170 DEG C, districts, three 180 DEG C, districts, four 180 DEG C, districts, five 180 DEG C, districts;
(3) by the injection moulding in parallel dual-screw injection moulding machine of step (2) gained pellet, temperature is 150 DEG C, a district, two 170 DEG C, districts, three 180 DEG C, districts, four 180 DEG C, districts, five 180 DEG C, districts.
The present embodiment product test the results are shown in table 1.
Embodiment 4
Molybdenumdisulphide pre-treatment step is as follows:
(1) molybdenumdisulphide of 4kg is joined in the dilution heat of sulfuric acid of 16wt% of 6L, it is heated to 70 DEG C, stir 2 hours, filter, with deionized water wash to neutral;Concentration molybdenumdisulphide after removal trace impurity being joined 7L is the sodium hydroxide solution of 16wt%, 70 DEG C, stirs 1.5 hours, filters, with deionized water wash to neutral, dry;
(2) concentration that pretreated molybdenumdisulphide adds 7L is in monoalkoxy lipid acid titanate coupling agent (titanate coupling agent UP-131) ethanolic soln of 0.8wt%, infiltrates 45 minutes, filters, and dries, obtains pretreated molybdenumdisulphide.
The preparation process of improved polyoxymethylene composite is as follows:
Raw material weight proportioning is: polyoxymethylene 95 parts, pretreated molybdenumdisulphide 5 parts, trimeric cyanamide 0.1 part, Zinic stearas 0.5 part.
Preparation method:
(1) raw material is weighed in proportion join in high-speed mixer, mixing 10min;
(2) by step (1) gained mixture at equidirectional parallel double-screw extruder extruding pelletization, temperature is 150 DEG C, a district, two 170 DEG C, districts, three 180 DEG C, districts, four 180 DEG C, districts, five 180 DEG C, districts;
(3) by the injection moulding in parallel dual-screw injection moulding machine of step (2) gained pellet, temperature is 150 DEG C, a district, two 170 DEG C, districts, three 180 DEG C, districts, four 180 DEG C, districts, five 180 DEG C, districts.
Its frictional coefficient and Volume erosion rate are tested by the polyformaldehyde composite material prepared by embodiment 1-4 above according to testing standard, and get pure polyoxymethylene as a comparison, and concrete testing standard and result are as shown in table 1 below:
Table 1: performance test
By upper table 1 test result it may be seen that polyformaldehyde composite material prepared by the present invention has excellent wear-resisting and lubricity; And comparing with pure polyoxymethylene, its wear resisting property improves greatly.
The above-mentioned description to embodiment can understand and apply the invention for ease of those skilled in the art. These embodiments obviously easily can be made various amendment by person skilled in the art, and General Principle described herein are applied in other embodiments and need not pass through creative work. Therefore, the invention is not restricted to embodiment here, those skilled in the art, according to the announcement of the present invention, do not depart from improvement that category of the present invention makes and amendment all should within protection scope of the present invention.
Claims (7)
1. an improved polyoxymethylene composite, it is characterised in that: it is made up by weight of following raw material:
Polyoxymethylene 80-95 part
Pretreated molybdenumdisulphide 5-20 part
Thermo-stabilizer 0.1��2.0 part
Lubricant 0.5-1.0 part.
2. improved polyoxymethylene composite according to claim 1, it is characterised in that: described pretreated molybdenumdisulphide adopts following step method to obtain:
(1) molybdenumdisulphide of 1-10kg is joined in the dilution heat of sulfuric acid of 15wt%-20wt% of 5-10L, it is heated to 50-80 DEG C, stir 1-2 hour, filter, with deionized water wash to neutral; It is the sodium hydroxide solution of 15wt%-20wt% that molybdenumdisulphide after trace impurity is removed in washing joins the concentration of 5-10L, 50-80 DEG C, stirs 1-2 hour, filters, with deionized water wash to neutral, dry;
(2) dried molybdenumdisulphide is added in the ethanolic soln of titanate coupling agent of 5-10L, infiltrate 30-60 minute, filter, dry, obtain pretreated molybdenumdisulphide; The ethanol solution concentration of described titanate coupling agent is 0.1wt%-1wt%.
3. improved polyoxymethylene composite according to claim 1, it is characterised in that: described molybdenumdisulphide purity >=98%, median size 10nm, specific surface area 200m2/g.
4. improved polyoxymethylene composite according to claim 1, it is characterised in that: the melting index of described polyoxymethylene is 9g/10min.
5. improved polyoxymethylene composite according to claim 1, it is characterised in that: described thermo-stabilizer is at least one in trimeric cyanamide, polymeric amide, Hinered phenols antioxidant.
6. improved polyoxymethylene composite according to claim 1, it is characterised in that: described lubricant is at least one of white oil, silicone oil, paraffin, stearic acid, calcium stearate, Zinic stearas.
7. the preparation method of improved polyoxymethylene composite described in the arbitrary item of claim 1-6, it is characterised in that: comprise the following steps:
(1) raw material is weighed in proportion join in high-speed mixer, mixing 2-10min;
(2) by step (1) gained mixture at equidirectional parallel double-screw extruder extruding pelletization, temperature is 150-180 DEG C;
(3) by the injection moulding in parallel dual-screw injection moulding machine of step (2) gained pellet, temperature is 150-180 DEG C.
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Cited By (2)
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| CN109694543A (en) * | 2018-12-06 | 2019-04-30 | 万华化学集团股份有限公司 | A kind of polyacetal composition and preparation method thereof |
| CN112831152A (en) * | 2021-01-10 | 2021-05-25 | 深圳市富恒新材料股份有限公司 | High-performance wear-resistant POM composite material and preparation method thereof |
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| CN109694543B (en) * | 2018-12-06 | 2022-01-07 | 万华化学集团股份有限公司 | Polyacetal composition and preparation method thereof |
| CN112831152A (en) * | 2021-01-10 | 2021-05-25 | 深圳市富恒新材料股份有限公司 | High-performance wear-resistant POM composite material and preparation method thereof |
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