CN104403771A - Heat resistant lubricant used for drawing refractory metal and preparation method thereof - Google Patents
Heat resistant lubricant used for drawing refractory metal and preparation method thereof Download PDFInfo
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- CN104403771A CN104403771A CN201410514378.3A CN201410514378A CN104403771A CN 104403771 A CN104403771 A CN 104403771A CN 201410514378 A CN201410514378 A CN 201410514378A CN 104403771 A CN104403771 A CN 104403771A
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Abstract
The invention discloses a heat resistant lubricant used for drawing refractory metal and a preparation method thereof. The heat resistant lubricant comprises the following components by weight: 10-30% of graphite, 0.1-2% of dispersant, 0.3-5% of thickening agent, 0.1-15% of emulsifier, 0.5-10% of film forming agent, 2-5% of ammoniacal liquor with concentration of 25%, 0.1-1% of antiseptic, 0.1-2% of adhesive, 0.3-3% of surfactant and balance of water. The heat resistant lubricant has good adhesive force under high temperature and can not generate explosion and shedding, lubricity, thermal conductivity and surface antioxidation performance between the drawing material and a mold can be effectively increased, heat due to friction can be reduced, and usage life of the mold can be prolonged.
Description
Technical field
The present invention relates to additive used in metallic high temperature wire-drawing technology field hard to tolerate, be specifically related to a kind of refractory metal drawing fire-resistant lubricants and preparation method thereof.
Background technology
Metal drawing imposes pulling force to metal stock, and making it by nib to obtain the plastic processing method with nib sectional dimension, goods that shape is identical, is the main method of production tubing, bar, section bar and wire rod.Metal drawing mode is divided into cold-drawn, hot drawing and temperature according to the temperature of metal during drawing and pulls out; Wherein cold-drawn be wire, metal wire produce in the mode of producing, be applicable to the metallic substance that fusing point is low, ductility is good; In hot drawing technique, wire needs heating before entering nib, is mainly used for refractory metal as tungsten, the drawing process of the metals such as molybdenum; And temperature when pulling out wire also need the temperature being heated to specify just to enter nib, be mainly used for zinc, difficult distortion alloy as the drawing of High Speed Steel Wire, bearing steel wire.The energy major part of usual drawing machining consumption is all in the friction of mould and drawable material, causes the rising of section temperature, failure of lubricating film easily occurs and even sinters.Therefore in drawing process, keep good lubricating status can reduce the heat rubbing and produce, contribute to the life-span extending mould, and guarantee not break in drawing process.Along with the raising of drawing speed, also more and more higher to the requirement of lubricant.
At present, in high temperature drawing process, the general aquadag that adopts makes lubricant.In high temperature drawing process, temperature is all between 400-1200 DEG C, the aquadag adopted is all make membrane-forming agent with syrup and agar, easily burst under high temperature and come off, causing the large generation of frictional force between drawable material and mould fracture of wire, scuffing, the deficiency such as string diameter consistence is poor, good article rate is low and mould loss is large.
Summary of the invention
In order to overcome the defect of prior art, of the present invention being provides a kind of refractory metal drawing fire-resistant lubricants, at high temperature there is good sticking power, there will not be explosion and come off, oilness, thermal conductivity and surface oxidation-resistant between effective raising drawable material and mould, reduce the heat rubbing and produce, extend the mold use life-span.
Another object of the present invention is to the preparation method that a kind of refractory metal drawing fire-resistant lubricants is provided, obtain a kind of fire-resistant lubricants by special process, effective oilness, thermal conductivity and the surface oxidation-resistant improved between drawable material and mould.
The technical solution adopted in the present invention is as follows for achieving the above object:
A kind of refractory metal drawing fire-resistant lubricants, it is prepared from by following raw material by weight percentage:
Graphite Powder 99 10-30%
Dispersion agent 0.1-2%
Thickening material 0.3-5%
Emulsifying agent 0.1-15%
Membrane-forming agent 0.5-10%
25% ammoniacal liquor 2-5%
Sanitas 0.1-1%
Tackiness agent 0.1-2%
Tensio-active agent 0.3-3%
The water yield is mended to a hundred per cent.
As preferred embodiments of the present invention, described emulsifying agent be one or both mixing in Starso or tween; Described thickening material is one or both mixing in sodium alginate or polyvinyl alcohol; Described dispersion agent is one or both mixing in Xylo-Mucine, sodium hydroxyethyl cellulose, methylcellulose gum, Vltra tears, hydroxyethylmethyl-cellulose; Described membrane-forming agent is styrene acrylic emulsion; Described sanitas is 5,5-dimethyl hydantion; Described tackiness agent is polyoxyethylene glycol; Described tensio-active agent is sodium metnylene bis-naphthalene sulfonate.
Adopt macromolecule emulsion to make membrane-forming agent in the present invention, make graphite granule form the drawing film of one deck densification on silk surface.
As the preferred scheme of one of the present invention, described refractory metal drawing fire-resistant lubricants is prepared from by following raw material by weight percentage:
Graphite Powder 99 10-30%, Xylo-Mucine 0.1-2%, polyvinyl alcohol 0.5-2%, tween 0.1-1%, styrene acrylic emulsion 0.5-10%, 25% ammoniacal liquor 2-5%, 5,5-dimethyl hydantion 0.1-1%, polyoxyethylene glycol 0.1-2%, sodium methylene bis-naphthalene sulfonate 0.3-3%, Starso 0.1-10%, sodium alginate 0.8%, the water yield are mended to a hundred per cent.
By the particle diameter controlling graphite, the content of impurity falls in the present invention.Preferably, the particle diameter of described Graphite Powder 99 is 0.15-1.2 μm.
A preparation method for refractory metal drawing fire-resistant lubricants, is characterized in that, its concrete steps are as follows:
1) Graphite Powder 99 is prepared
Pulverize: natural flake graphite is carried out case of wet attrition after comminution by gas stream;
Classification: the Graphite Powder 99 after pulverizing adopts horizontal pre-sorting machine to carry out centrifugal classification, filters out particle diameter and is less than the graphite particle of 5 μm again through smart extension set 5000-6000 rev/min of high speed centrifugation separation, obtain the graphite particle that particle diameter is less than 1.2 μm;
Purify: first above-mentioned graphite slurries are added in reactor, start reactor stirrer, add 30% technical hydrochloric acid by sour pump while stirring, and use water flushing pipeline; Leave standstill after continuously stirring, then with pump, the material in reactor is squeezed in pressure filter, and be washed to pH value 7-8, isolate filter cake stand-by.
2) according to formula ratio in above-mentioned steps 1) process after Graphite Cake in add ammoniacal liquor, dispersion agent and part water, high-speed stirring is uniformly dispersed, membrane-forming agent, emulsifying agent, thickening material, sanitas, tensio-active agent, tackiness agent and remaining water is added again according to formula ratio, ball milling in ball mill is squeezed into by air pump after high speed dispersion, stir after discharge.
In aforesaid method, step 1) in case of wet attrition be adopt Z-30 type ball mill circulation pearl mill 15-25 hour.
In aforesaid method, step 1) filter out in classification process >=graphite particle of 5 μm is transferred to Z-30 type ball mill circulation pearl mill, and then successively through purifying, washing, press filtration step, repeat with this.
Compared to existing technology, beneficial effect of the present invention is:
1. the present invention to adopt through the natural flake graphite of comminution by gas stream again through meticulous case of wet attrition technique and chemical purification technique, makes graphite particle size D50 between 0.15-1.2um, can formulate different size-grade distribution and foreign matter content is lower according to the string diameter difference drawn;
2. the present invention adopts macromolecule emulsion to make membrane-forming agent, graphite granule is made to form the drawing film of one deck densification on silk surface, do painting film adhesive with Starso, under high temperature, sticking power there will not be well explosion and comes off, and effectively improves the oilness of silk and mould, thermal conductivity and surface oxidation-resistant;
3. refractory metal drawing fire-resistant lubricants of the present invention has optimum dispersion state, and can keep stable for a long time under high temperature, does not condense, does not precipitate, not corrupt, not skinning, keeps use procedure uniformity consistency;
4. refractory metal drawing fire-resistant lubricants of the present invention can make the utilization ratio of wire drawing diamond mould greatly improve, and can improve 30-50%.
Below in conjunction with concrete embodiment, the present invention is described in further detail.
Embodiment
Embodiment 1
A kind of refractory metal drawing fire-resistant lubricants, it is prepared from by following raw material by weight percentage:
Graphite 12%, polyvinyl alcohol 0.6%, Xylo-Mucine 0.55%, tween 0.1%, styrene acrylic emulsion 6%, polyoxyethylene glycol 2%, Starso 5%, 5,5-dimethyl hydantion 0.3%, ammoniacal liquor 4%, pure water are mended to a hundred per cent;
Its preparation technology is as follows:
1) Graphite Powder 99 is prepared
Pulverize: after comminution by gas stream, adopted by natural flake graphite Z-30 type ball mill circulation pearl to grind carry out case of wet attrition in 15-25 hour;
Classification: the Graphite Powder 99 after pulverizing adopts horizontal pre-sorting machine to carry out centrifugal classification, filters out the graphite particle that particle diameter is less than 5 μm and is separated through smart extension set 5000-6000 rev/min of high speed centrifugation, obtains the graphite particle of particle diameter D50≤0.5 μm;
Purify: first above-mentioned graphite slurries are added in reactor, start reactor stirrer, add 30% technical hydrochloric acid by sour pump while stirring, and use water flushing pipeline; Leave standstill after continuously stirring, then with pump, the material in reactor is squeezed in pressure filter, and be washed to pH value 7-8, isolate filter cake stand-by;
2) according to formula ratio in above-mentioned steps 1) process after Graphite Cake in add ammoniacal liquor, dispersion agent and part water, high-speed stirring is uniformly dispersed, styrene acrylic emulsion, 5 is added again according to formula ratio, 5-dimethyl hydantion, Starso, polyoxyethylene glycol, tween, polyvinyl alcohol and remaining water, ball milling in ball mill is squeezed into by air pump after high speed dispersion, stir after discharge.
Embodiment 2
A kind of refractory metal drawing fire-resistant lubricants, it is prepared from by following raw material by weight percentage:
Graphite 19%, sodium methylene bis-naphthalene sulfonate 0.5%, sodium alginate 0.7%, Xylo-Mucine 0.75%, polyoxyethylene glycol 2.6%, 5,5-dimethyl hydantion 0.3%, ammoniacal liquor 4.5%, Starso 8%, pure water are mended to a hundred per cent;
Its preparation technology is as follows:
1) Graphite Powder 99 is prepared
Pulverize: after comminution by gas stream, adopted by natural flake graphite Z-30 type ball mill circulation pearl to grind carry out case of wet attrition in 15-25 hour;
Classification: the Graphite Powder 99 after pulverizing adopts horizontal pre-sorting machine to carry out centrifugal classification, filters out the graphite particle that particle diameter is less than 5 μm and is separated through smart extension set 5000-6000 rev/min of high speed centrifugation, obtains the graphite particle of particle diameter D50≤0.8 μm;
Purify: first above-mentioned graphite slurries are added in reactor, start reactor stirrer, add 30% technical hydrochloric acid by sour pump while stirring, and use water flushing pipeline; Leave standstill after continuously stirring, then with pump, the material in reactor is squeezed in pressure filter, and be washed to pH value 7-8, isolate filter cake;
2) according to formula ratio in above-mentioned steps 1) process after Graphite Cake in add ammoniacal liquor, dispersion agent and part water, high-speed stirring is uniformly dispersed, sodium methylene bis-naphthalene sulfonate, sodium alginate, polyoxyethylene glycol, Starso, 5 is added again according to formula ratio, 5-dimethyl hydantion and remaining water, ball milling in ball mill is squeezed into by air pump after high speed dispersion, stir after discharge.
Embodiment 3
A kind of refractory metal drawing fire-resistant lubricants, it is prepared from by following raw material by weight percentage:
Graphite 22%, sodium methylene bis-naphthalene sulfonate 0.6%, Xylo-Mucine 0.65%, sodium alginate 0.68, polyvinyl alcohol 0.5%, polyoxyethylene glycol 3%, 5,5-dimethyl hydantion 0.5%, ammoniacal liquor 5%, Starso 10%, pure water are mended to a hundred per cent;
Its preparation technology is as follows:
1) Graphite Powder 99 is prepared
Pulverize: after comminution by gas stream, adopted by natural flake graphite Z-30 type ball mill circulation pearl to grind carry out case of wet attrition in 15-25 hour;
Classification: the Graphite Powder 99 after pulverizing adopts horizontal pre-sorting machine to carry out centrifugal classification, filters out the graphite particle that particle diameter is less than 5 μm and is separated through smart extension set 5000-6000 rev/min of high speed centrifugation, obtains the graphite particle of particle diameter D50≤1.2 μm;
Purify: first above-mentioned graphite slurries are added in reactor, start reactor stirrer, add 30% technical hydrochloric acid by sour pump while stirring, and use water flushing pipeline; Leave standstill after continuously stirring, then with pump, the material in reactor is squeezed in pressure filter, and be washed to pH value 7-8, isolate filter cake stand-by;
2) according to formula ratio in above-mentioned steps 1) process after Graphite Cake in add ammoniacal liquor, dispersion agent and part water, high-speed stirring is uniformly dispersed, Starso, sodium alginate, sodium methylene bis-naphthalene sulfonate, polyoxyethylene glycol, 5 is added again according to formula ratio, 5-dimethyl hydantion, polyvinyl alcohol and remaining water, ball milling in ball mill is squeezed into by air pump after high speed dispersion, stir after discharge.
Performance Detection
1. the dried Components identification of refractory metal drawing fire-resistant lubricants of above-described embodiment 1-3, the results are shown in Table 1.
Table 1
| Numbering | Dry residue (%) | Graphite (%) | Ash (%) | Iron level ppm |
| Embodiment 1 | ≥18.0 | ≥13.5 | ≤2.0 | ≤250 |
| Embodiment 2 | ≥21.0 | ≥17.5 | ≤2.0 | ≤200 |
| Embodiment 3 | ≥25.0 | ≥21.0 | ≤2.0 | ≤200 |
2. detect the refractory metal drawing fire-resistant lubricants outward appearance of above-described embodiment 1-3, smell, pH value, stability, granularity, sticking power according to standard Q/TR1-026-1998, detected result is in table 2.
Table 2
Sticking power: adopt the method for drawing lattice experiment, the printing layer of ink utilizing adhesion-force tester to test to make with above-mentioned ink is to the adhesion property of base material, in the 3M adhesive tape sticking adopting 20mm wide printing layer of ink after hardening, take off with minimum angles, conductive film layer adhesive power is divided into 0 ~ 5 grade.Wherein 0 grade is greater than 95% for the lubricant layer be attached on adhesive tape, and 1 grade is greater than 50%, and 2 grades are less than 30%, and 3 grades are less than 20%, and 4 grades are less than 10%, and 5 grades are less than 2%.
Above-mentioned embodiment is only the preferred embodiment of the present invention; can not limit the scope of protection of the invention with this, change and the replacement of any unsubstantiality that those skilled in the art does on basis of the present invention all belong to the present invention's scope required for protection.
Claims (7)
1. a refractory metal drawing fire-resistant lubricants, is characterized in that, it is prepared from by following raw material by weight percentage:
Graphite Powder 99 10-30%
Dispersion agent 0.1-2%
Thickening material 0.3-5%
Emulsifying agent 0.1-15%
Membrane-forming agent 0.5-10%
25% ammoniacal liquor 2-5%
Sanitas 0.1-1%
Tackiness agent 0.1-2%
Tensio-active agent 0.3-3%
The water yield is mended to a hundred per cent.
2. refractory metal drawing fire-resistant lubricants according to claim 1, is characterized in that,
Described emulsifying agent is one or both mixing in Starso or tween;
Described thickening material is one or both mixing in sodium alginate or polyvinyl alcohol;
Described dispersion agent is one or both mixing in Xylo-Mucine, sodium hydroxyethyl cellulose, methylcellulose gum, Vltra tears, hydroxyethylmethyl-cellulose;
Described membrane-forming agent is styrene acrylic emulsion;
Described sanitas is 5,5-dimethyl hydantion;
Described tackiness agent is polyoxyethylene glycol;
Described tensio-active agent is sodium metnylene bis-naphthalene sulfonate.
3. refractory metal drawing fire-resistant lubricants according to claim 2, is characterized in that, it is prepared from by following raw material by weight percentage:
Graphite Powder 99 10-30%, Xylo-Mucine 0.1-2%, polyvinyl alcohol 0.5-2%, tween 0.1-1%, styrene acrylic emulsion 0.5-10%, 25% ammoniacal liquor 2-5%, 5,5-dimethyl hydantion 0.1-1%, polyoxyethylene glycol 0.1-2%, sodium metnylene bis-naphthalene sulfonate 0.3-3%, Starso 0.1-10%, sodium alginate 0.8%, the water yield are mended to a hundred per cent.
4. refractory metal drawing fire-resistant lubricants according to claim 3, is characterized in that, the particle diameter of described Graphite Powder 99 is 0.15-1.2 μm.
5. the preparation method of the refractory metal drawing fire-resistant lubricants as described in any one of claim 1-4, it is characterized in that, its concrete steps are as follows:
1) Graphite Powder 99 is prepared
Pulverize: natural flake graphite is carried out case of wet attrition after comminution by gas stream;
Classification: the Graphite Powder 99 after pulverizing adopts horizontal pre-sorting machine to carry out centrifugal classification, filters out particle diameter and is less than the graphite particle of 5 μm again through smart extension set 5000-6000 rev/min of high speed centrifugation separation, obtain the graphite particle that particle diameter is less than 1.2 μm;
Purify: first above-mentioned graphite slurries are added in reactor, start reactor stirrer, add 30% technical hydrochloric acid by sour pump while stirring, and use water flushing pipeline; Leave standstill after continuously stirring, then with pump, the material in reactor is squeezed in pressure filter, and be washed to pH value 7-8, isolate filter cake stand-by.
2) according to formula ratio in above-mentioned steps 1) process after Graphite Cake in add ammoniacal liquor, dispersion agent and part water, high-speed stirring is uniformly dispersed, thickening material, emulsifying agent, membrane-forming agent, sanitas, tensio-active agent, tackiness agent and remaining water is added again according to formula ratio, ball milling in ball mill is squeezed into by air pump after high speed dispersion, stir after discharge.
6. preparation method according to claim 5, is characterized in that, step 1) in case of wet attrition be adopt Z-30 type ball mill circulation pearl mill 15-25 hour.
7. preparation method according to claim 6, is characterized in that, step 1) filter out in classification process >=graphite particle of 5 μm is transferred to Z-30 type ball mill circulation pearl mill, and then successively through purifying, washing, press filtration step, repeat with this.
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| CN104962367A (en) * | 2015-07-20 | 2015-10-07 | 广西大学 | Thick niobium wire drawing lubricant composition |
| CN106701291A (en) * | 2016-12-16 | 2017-05-24 | 池州市旭豪机械有限公司 | Water-soluble cold drawing steel pipe lubricant |
| CN106867648A (en) * | 2016-12-22 | 2017-06-20 | 当涂县宏宇金属炉料有限责任公司 | A kind of waste lubricating oil makes wire drawing powder method |
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| CN107723067A (en) * | 2017-10-26 | 2018-02-23 | 湖南金化科技集团有限公司 | A kind of water-based low temperature resistant graphitic lubricant and its preparation method and application |
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- 2014-09-29 CN CN201410514378.3A patent/CN104403771A/en active Pending
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| CN104962367A (en) * | 2015-07-20 | 2015-10-07 | 广西大学 | Thick niobium wire drawing lubricant composition |
| CN106701291A (en) * | 2016-12-16 | 2017-05-24 | 池州市旭豪机械有限公司 | Water-soluble cold drawing steel pipe lubricant |
| CN106867648A (en) * | 2016-12-22 | 2017-06-20 | 当涂县宏宇金属炉料有限责任公司 | A kind of waste lubricating oil makes wire drawing powder method |
| CN106867648B (en) * | 2016-12-22 | 2020-04-21 | 当涂县宏宇金属炉料有限责任公司 | Method for preparing wire drawing powder from waste lubricating oil |
| CN107603725A (en) * | 2017-10-08 | 2018-01-19 | 六安市九十里山水画廊有限公司 | Handicraft surface baste agitator anti-stick lubricates liquid and preparation method thereof |
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| CN110591420B (en) * | 2019-08-09 | 2021-04-02 | 青岛久益石墨有限公司 | Metal plate conveying release agent and preparation method thereof |
| CN110591420A (en) * | 2019-08-09 | 2019-12-20 | 青岛久益石墨有限公司 | Metal plate conveying release agent and preparation method thereof |
| CN111286398A (en) * | 2020-04-18 | 2020-06-16 | 沈阳名华时代科技有限公司 | Formula and production process of automotive forged graphite type release agent |
| CN111909766A (en) * | 2020-07-15 | 2020-11-10 | 浙江机电职业技术学院 | High-fluidity lubricant for metal drawing and application thereof |
| CN111909766B (en) * | 2020-07-15 | 2022-03-15 | 浙江机电职业技术学院 | High-fluidity lubricant for metal drawing and application thereof |
| CN111778093A (en) * | 2020-08-05 | 2020-10-16 | 陕西高精尖新材料科技有限责任公司 | Titanium alloy wire high-temperature drawing oil-based lubricant and preparation method thereof |
| CN111849600A (en) * | 2020-08-05 | 2020-10-30 | 陕西高精尖新材料科技有限责任公司 | Titanium alloy wire high-temperature drawing dry-type lubricant and preparation method thereof |
| CN113399483A (en) * | 2021-06-07 | 2021-09-17 | 威海银兴预应力线材有限公司 | Environment-friendly lubricating coating agent for cold-drawn steel wire and preparation method and application thereof |
| CN114369494A (en) * | 2022-01-12 | 2022-04-19 | 赵利华 | Lubricating liquid for reducing die wear and preparation method thereof |
| CN116606683A (en) * | 2023-02-20 | 2023-08-18 | 铃木加普腾钢丝（苏州）有限公司 | Drawing powder for high-speed drawing process |
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