CN105647103B - A kind of improved polyoxymethylene composite and preparation method thereof - Google Patents
A kind of improved polyoxymethylene composite and preparation method thereof Download PDFInfo
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- CN105647103B CN105647103B CN201410627502.7A CN201410627502A CN105647103B CN 105647103 B CN105647103 B CN 105647103B CN 201410627502 A CN201410627502 A CN 201410627502A CN 105647103 B CN105647103 B CN 105647103B
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- molybdenum disulfide
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Abstract
The invention discloses a kind of improved polyoxymethylene composites, are made by weight of following raw material: 80-95 parts of polyformaldehyde, molybdenum disulfide 5-20 parts pretreated, 0.1~2.0 part of heat stabilizer, 0.5-1.0 parts of lubricant.Invention additionally discloses the preparation method of the improved polyoxymethylene composite, steps are as follows: (1) weighs raw material in proportion and be added in high-speed mixer, mix 2-10min；(2) by mixture obtained by step (1) in equidirectional parallel double-screw extruder extruding pelletization, temperature is 150-180 DEG C；(3) by pellet injection molding in parallel dual-screw injection molding machine obtained by step (2), temperature is 150-180 DEG C.Polyformaldehyde composite material produced by the present invention has the excellent properties of wear-resisting lubrication, can be widely used in modifying plastics field.
Description
Technical field
The present invention relates to polymeric material field more particularly to a kind of improved polyoxymethylene composite and its preparation processes.
Background technique
Polyformaldehyde is a kind of engineering plastics of high comprehensive performance, has high strength and stiffness, and good size is steady
Qualitative, excellent fatigue durability, creep resistant, self-lubrication and wear-resisting property, in machinery, automobile, electronics, household electrical appliances and building materials etc.
Aspect is widely used in the various parts with low frictional coefficient wearable performance of manufacture.But the thermal stability of polyformaldehyde at high temperature is poor, easy
It decomposes；And its machine-shaping temperature is narrow, and resistance to ag(e)ing is poor, is only capable of using under conditions of low speed, underload.In order to make poly- first
Aldehyde uses under the harsh conditions such as high speed, high load capacity, just must be on the basis of original excellent physical mechanical property, further
Its coefficient of friction and wear rate are reduced, this just needs to realize by the modification of polyformaldehyde.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the shortcomings of existing polyformaldehyde material, provide a kind of low frictional coefficient wearable, system
Standby simple process, lower-cost improved polyoxymethylene composite and preparation method thereof.
The present invention solves technical solution used by told technical problem:
A kind of improved polyoxymethylene composite is made by weight of following raw material:
80-95 parts of polyformaldehyde
Pretreated molybdenum disulfide 5-20 parts
0.1~2.0 part of heat stabilizer
0.5-1.0 parts of lubricant
The pretreated molybdenum disulfide is obtained using following step method:
(1) molybdenum disulfide of 1-10kg is added in the dilution heat of sulfuric acid of 15wt%-20wt% of 5-10L, is heated to 50-
It 80 DEG C, stirs 1-2 hours, filtering is washed with deionized to neutrality；Molybdenum disulfide after washing being removed trace impurity is added
The sodium hydroxide solution that concentration to 5-10L is 15wt%-20wt%, is stirred 1-2 hours by 50-80 DEG C, and deionized water is used in filtering
Washing is dry to neutrality；
(2) molybdenum disulfide after drying is added in the ethanol solution of titanate coupling agent of 5-10L, 30-60 points of infiltration
Clock filters, and drying obtains pretreated molybdenum disulfide；The ethanol solution concentration of the titanate coupling agent is 0.1wt%-
1wt%。
Wherein, the purpose of the step (1) is: 1, removing molybdenum disulfide surface impurity；2, slight erosion molybdenum disulfide table
Face increases the roughness on molybdenum disulfide surface, improves the compatibility and mechanical property of polymer.Dilute sulfuric acid and sodium hydroxide solution
Concentration, heating temperature are excessively high or the too long meeting heavy corrosion molybdenum disulfide of mixing time can even dissolve molybdenum disulfide, big havoc
The performance of molybdenum disulfide itself；Concentration, heating temperature are too low, mixing time is short, do not have the due effect of the step.
Step (2) described titanate coupling agent can be titanate coupling agent UP-131.
Molybdenum disulfide purity >=98%, 10 nm of average grain diameter, 200 m2/g of specific surface area.Here partial size with than
Surface area cannot be too small, too small to cause serious reunion between powder；Can not be too big, too big partial size can be such that compatibility becomes
Difference.After soda acid is handled, degree of being corroded is also relatively good for this partial size and the diamond of specific surface area, after coupling agent treatment, energy
The wearability and other mechanical properties of the raising composition of amplitude peak.
Further, the melt index of the polyformaldehyde is 9g/10min.
Further, the heat stabilizer is at least one of melamine, polyamide, Hinered phenols antioxidant.Wherein
Hinered phenols antioxidant includes antioxidant 1010 (four [methyl-β-(3,5- di-tert-butyl-hydroxy phenyl) propionic ester] Ji Wusi
Alcohol ester), irgasfos 168 (three [ 2.4- di-tert-butyl-phenyl ] phosphite esters).
Further, the lubricant is at least one of white oil, silicone oil, paraffin, stearic acid, calcium stearate, zinc stearate.
Another technical solution of the invention is to provide the preparation method of above-mentioned improved polyoxymethylene composite, including following step
It is rapid:
(1) raw material is weighed in proportion and is added in high-speed mixer, mix 2-10min；
(2) by mixture obtained by step (1) in equidirectional parallel double-screw extruder extruding pelletization, temperature is 150-180 DEG C；
(3) by pellet injection molding in parallel dual-screw injection molding machine obtained by step (2), temperature is 150-180 DEG C.
Polyformaldehyde composite material produced by the present invention has the excellent properties of wear-resisting lubrication, can be widely used in plastics
Modified field.
Specific embodiment
Invention is further described in detail with reference to embodiments.
Embodiment 1
Molybdenum disulfide pre-treatment step is as follows:
(1) molybdenum disulfide of 1kg is added in the dilution heat of sulfuric acid of 15wt% of 5L, is heated to 50 DEG C, stirred 1 hour,
Filtering, is washed with deionized to neutrality；The hydrogen for being 15wt% the concentration that the molybdenum disulfide after removal trace impurity is added to 5L
Sodium hydroxide solution 50 DEG C, stirs 1 hour, filtering, is washed with deionized to neutrality, dry；
(2) ethyl alcohol for the titanate coupling agent UP-131 for being 0.1wt% by the concentration that 5L is added in pretreated molybdenum disulfide
It in solution, infiltrates 30 minutes, filters, drying obtains pretreated molybdenum disulfide.
The preparation step of improved polyoxymethylene composite is as follows:
Raw material weight proportioning of soup processed are as follows: 90 parts of polyformaldehyde, 10 parts of pretreated molybdenum disulfide, 1 part of antioxidant 1010, antioxidant
168 1 parts, 0.5 part of silicone oil, 0.5 part of calcium stearate.
(1) above-mentioned raw materials are weighed in proportion and is added in high-speed mixer, mix 5min；
(2) by mixture obtained by step (1) in equidirectional parallel double-screw extruder extruding pelletization, temperature is 150 DEG C of an area,
Two 170 DEG C of areas, three 180 DEG C of areas, four 180 DEG C of areas, five 180 DEG C of areas；
(3) by pellet injection molding in parallel dual-screw injection molding machine obtained by step (2), temperature is 150 DEG C of an area, 2nd area
170 DEG C, three 180 DEG C of areas, four 180 DEG C of areas, five 180 DEG C of areas.The present embodiment products obtained therefrom performance test methods standard number and survey
Test result is listed in table 1.
Embodiment 2
Molybdenum disulfide pre-treatment step is as follows:
(1) molybdenum disulfide of 2kg is added in the dilution heat of sulfuric acid of 18 wt % of 6L, is heated to 60 DEG C, stirring 1.5
Hour, filtering is washed with deionized to neutrality；It is 18 the concentration that the molybdenum disulfide after removal trace impurity is added to 8L
The sodium hydroxide solution of wt % 60 DEG C, stirs 1.5 hours, filtering, is washed with deionized to neutrality, dry；
(2) the monoalkoxy fatty acid titanate esters idol for being 0.5 wt % by the concentration that 8L is added in pretreated molybdenum disulfide
Join in agent (titanate coupling agent UP-131) ethanol solution, infiltrate 40 minutes, filter, drying obtains pretreated molybdenum disulfide.
The preparation step of improved polyoxymethylene composite is as follows:
The present embodiment raw material weight proportioning of soup processed are as follows: 85 parts of polyformaldehyde, 15 parts of pretreated molybdenum disulfide, antioxidant 1010 0.1
Part, 0.5 part of silicone oil.
Preparation method:
(1) raw material is weighed in proportion and is added in high-speed mixer, mix 2min；
(2) by mixture obtained by step (1) in equidirectional parallel double-screw extruder extruding pelletization, temperature is 150 DEG C of an area,
Two 170 DEG C of areas, three 180 DEG C of areas, four 180 DEG C of areas, five 180 DEG C of areas；
(3) by pellet injection molding in parallel dual-screw injection molding machine obtained by step (2), temperature is 150 DEG C of an area, 2nd area
170 DEG C, three 180 DEG C of areas, four 180 DEG C of areas, five 180 DEG C of areas.
The present embodiment product test result is listed in table 1.
Embodiment 3
Molybdenum disulfide pre-treatment step is as follows:
(1) molybdenum disulfide of 10kg is added in the dilution heat of sulfuric acid of 20 wt % of 10L, is heated to 80 DEG C, stirring 2
Hour, filtering is washed with deionized to neutrality；It is 20 the concentration that the molybdenum disulfide after removal trace impurity is added to 10L
The sodium hydroxide solution of wt % 80 DEG C, stirs 2 hours, filtering, is washed with deionized to neutrality, dry；
(2) the monoalkoxy fatty acid titanate esters idol for being 1 wt % by the concentration that 10L is added in pretreated molybdenum disulfide
Join in agent (titanate coupling agent UP-131) ethanol solution, infiltrate 60 minutes, filter, drying obtains pretreated molybdenum disulfide.
The preparation step of improved polyoxymethylene composite is as follows:
Raw material weight proportioning of soup processed are as follows: 80 parts of polyformaldehyde, 20 parts of pretreated molybdenum disulfide, 1 part of antioxidant 1010, antioxidant
168 0.5 parts, 0.5 part of white oil, 0.5 part of paraffin.
Preparation method:
(1) raw material is weighed in proportion and is added in high-speed mixer, mix 8min；
(2) by mixture obtained by step (1) in equidirectional parallel double-screw extruder extruding pelletization, temperature is 150 DEG C of an area,
Two 170 DEG C of areas, three 180 DEG C of areas, four 180 DEG C of areas, five 180 DEG C of areas；
(3) by pellet injection molding in parallel dual-screw injection molding machine obtained by step (2), temperature is 150 DEG C of an area, 2nd area
170 DEG C, three 180 DEG C of areas, four 180 DEG C of areas, five 180 DEG C of areas.
The present embodiment product test result is listed in table 1.
Embodiment 4
Molybdenum disulfide pre-treatment step is as follows:
(1) molybdenum disulfide of 4kg is added in the dilution heat of sulfuric acid of 16 wt % of 6L, is heated to 70 DEG C, stirring 2 is small
When, filtering is washed with deionized to neutrality；It is 16 wt the concentration that the molybdenum disulfide after removal trace impurity is added to 7L
The sodium hydroxide solution of % 70 DEG C, stirs 1.5 hours, filtering, is washed with deionized to neutrality, dry；
(2) the monoalkoxy fatty acid titanate esters idol for being 0.8 wt % by the concentration that 7L is added in pretreated molybdenum disulfide
Join in agent (titanate coupling agent UP-131) ethanol solution, infiltrate 45 minutes, filter, drying obtains pretreated molybdenum disulfide.
The preparation step of improved polyoxymethylene composite is as follows:
Raw material weight proportioning of soup processed are as follows: 95 parts of polyformaldehyde, 5 parts of pretreated molybdenum disulfide, 0.1 part of melamine, zinc stearate
0.5 part.
Preparation method:
(1) raw material is weighed in proportion and is added in high-speed mixer, mix 10min；
(2) by mixture obtained by step (1) in equidirectional parallel double-screw extruder extruding pelletization, temperature is 150 DEG C of an area,
Two 170 DEG C of areas, three 180 DEG C of areas, four 180 DEG C of areas, five 180 DEG C of areas；
(3) by pellet injection molding in parallel dual-screw injection molding machine obtained by step (2), temperature is 150 DEG C of an area, 2nd area
170 DEG C, three 180 DEG C of areas, four 180 DEG C of areas, five 180 DEG C of areas.
Polyformaldehyde composite material prepared by example 1 above -4 wears its coefficient of friction and volume according to testing standard
Rate is tested, and takes pure polyformaldehyde as a comparison, and specific testing standard and result are as shown in table 1 below:
Table 1: performance test
By upper 1 test result of table can be seen that polyformaldehyde composite material prepared by the present invention have it is excellent it is wear-resisting with
Greasy property；And it is compared with pure polyformaldehyde, wear-resisting property greatly improves.
The above-mentioned description to embodiment is for that can understand and apply the invention convenient for those skilled in the art.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to embodiments here, originally
Field technical staff announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be in the present invention
Protection scope within.
Claims (5)
1. a kind of improved polyoxymethylene composite, it is characterised in that: be made by weight of following raw material:
80-95 parts of polyformaldehyde
Pretreated molybdenum disulfide 5-20 parts
0.1~2.0 part of heat stabilizer
0.5-1.0 parts of lubricant；
The pretreated molybdenum disulfide is obtained using following step method:
(1) molybdenum disulfide of 1-10kg is added in the dilution heat of sulfuric acid of 15wt%-20wt% of 5-10L, is heated to 50-80
DEG C, it stirs 1-2 hours, filtering is washed with deionized to neutrality；Molybdenum disulfide after washing being removed trace impurity is added to
The concentration of 5-10L is the sodium hydroxide solution of 15wt%-20wt%, 50-80 DEG C, is stirred 1-2 hours, and filtering is washed with deionized water
It washs to neutrality, it is dry；
(2) molybdenum disulfide after drying is added in the ethanol solution of titanate coupling agent of 5-10L, is infiltrated 30-60 minutes, mistake
Filter, drying, obtains pretreated molybdenum disulfide；The ethanol solution concentration of the titanate coupling agent is 0.1wt%-1wt%；
Molybdenum disulfide purity >=98%, average grain diameter 10nm, 200 m of specific surface area2/g。
2. improved polyoxymethylene composite according to claim 1, it is characterised in that: the melt index of the polyformaldehyde
For 9g/10min.
3. improved polyoxymethylene composite according to claim 1, it is characterised in that: the heat stabilizer is melamine
At least one of amine, polyamide, Hinered phenols antioxidant.
4. improved polyoxymethylene composite according to claim 1, it is characterised in that: the lubricant be white oil, silicone oil,
At least one of paraffin, stearic acid, calcium stearate, zinc stearate.
5. the preparation method of the described in any item improved polyoxymethylene composites of claim 1-4, it is characterised in that: including following
Step:
(1) raw material is weighed in proportion and is added in high-speed mixer, mix 2-10min；
(2) by mixture obtained by step (1) in equidirectional parallel double-screw extruder extruding pelletization, temperature is 150-180 DEG C；
(3) by pellet injection molding in parallel dual-screw injection molding machine obtained by step (2), temperature is 150-180 DEG C.
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| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101121809A (en) * | 2007-09-14 | 2008-02-13 | 上海材料研究所 | Lead-free modified polyformaldehyde material and its preparing method |
| CN103357425A (en) * | 2013-07-10 | 2013-10-23 | 黑龙江大学 | Preparation method of molybdenum disulfide/titanium dioxide composite material with nano thorn hierarchical structure |
| CN103756245A (en) * | 2011-10-20 | 2014-04-30 | 杨晓莉 | Modified polyformaldehyde material and preparation method thereof |
| CN104045965A (en) * | 2014-06-17 | 2014-09-17 | 合肥杰事杰新材料股份有限公司 | Micronized polytetrafluoroethylene wax modified polyformaldehyde composite material and preparation method thereof |
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2014
- 2014-11-10 CN CN201410627502.7A patent/CN105647103B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101121809A (en) * | 2007-09-14 | 2008-02-13 | 上海材料研究所 | Lead-free modified polyformaldehyde material and its preparing method |
| CN103756245A (en) * | 2011-10-20 | 2014-04-30 | 杨晓莉 | Modified polyformaldehyde material and preparation method thereof |
| CN103357425A (en) * | 2013-07-10 | 2013-10-23 | 黑龙江大学 | Preparation method of molybdenum disulfide/titanium dioxide composite material with nano thorn hierarchical structure |
| CN104045965A (en) * | 2014-06-17 | 2014-09-17 | 合肥杰事杰新材料股份有限公司 | Micronized polytetrafluoroethylene wax modified polyformaldehyde composite material and preparation method thereof |
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