CN107129857A - Wear-resisting environment-friendly type stop-leak compound of antirust and preparation method thereof - Google Patents

Wear-resisting environment-friendly type stop-leak compound of antirust and preparation method thereof Download PDF

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Publication number
CN107129857A
CN107129857A CN201710397106.3A CN201710397106A CN107129857A CN 107129857 A CN107129857 A CN 107129857A CN 201710397106 A CN201710397106 A CN 201710397106A CN 107129857 A CN107129857 A CN 107129857A
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wear
parts
friendly type
leak compound
antirust
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吴德斌
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Jiangsu Hok Seal Material Co Ltd
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Jiangsu Hok Seal Material Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/06Mixtures of thickeners and additives
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/10Materials in mouldable or extrudable form for sealing or packing joints or covers
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04Elements
    • C10M2201/041Carbon; Graphite; Carbon black
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/062Oxides; Hydroxides; Carbonates or bicarbonates
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08Inorganic acids or salts thereof
    • C10M2201/082Inorganic acids or salts thereof containing nitrogen
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/085Phosphorus oxides, acids or salts
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/026Butene
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02Hydroxy compounds
    • C10M2207/021Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/283Esters of polyhydroxy compounds
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/287Partial esters
    • C10M2207/289Partial esters containing free hydroxy groups
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2215/044Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms having cycloaliphatic groups
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/042Sulfate esters
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2223/00Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/06Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having phosphorus-to-carbon bonds
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/12Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/34Lubricating-sealants
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10Semi-solids; greasy

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Lubricants (AREA)

Abstract

The present invention discloses a kind of wear-resisting environment-friendly type stop-leak compound of antirust, is made up of universal lithium base grease, tackifier, corrosion inhibiter, complex calcium phosphate, environmentally friendly expanded graphite and polytetrafluoroethylene (PTFE).Compared with prior art, compared with prior art, the environment-friendly type stop-leak compound that the antirust of the present invention is wear-resisting introduces sustained release agent and complex calcium phosphate respectively, make it have multiple anti-rust action, complex calcium phosphate is slightly soluble in water under corrosive environment atmosphere, very strong to the chelating ability of metal, in iron surface formation passive state envelope, with excellent rust-proof effect, environmental protection;The environmentally friendly expanded graphite of introducing not sulfur-bearing (or low-sulfur), with highly expanded rate, good corrosion resistance, anti-wear performance is good;The environment-friendly type stop-leak compound that the antirust of the present invention is wear-resisting is different from conventional seals fat, with preferably anti-wiping property and corrosion resistance, risk of the heavy metal to environment is reduced without zinc powder on the premise of thread compound performance is ensured in addition, the Health cost to user is reduced, with environment friendly.

Description

Wear-resisting environment-friendly type stop-leak compound of antirust and preparation method thereof
Technical field
The present invention relates to lubrication and sealing material field, the wear-resisting environment-friendly type stop-leak compound of more particularly to a kind of antirust and its system Preparation Method.
Background technology
Oil stop-leak compound is special tubing string lubrication and a kind of used important materials of sealing during oil exploitation, due to Use environment severe (such as extremely cold, very hot, wet or dry, dirty, high corrosion environment) can cause the viscous plug oil circuit of button, shackle, hand Apply the problems such as operation difficulty, screw corrosion, environmental pollution.The research and development technology of external thread sealing grease better than the country, sealing, There is unified standard, external thread compound occupies most of share of China market in terms of friction and tightening degree.
The defect of prior art:The thread sealing grease generally used at present is unstable in corrosion-resistant crocking resistance, and The heavy metals such as addition lead powder, zinc powder are needed, have larger harm to environment and human body.Domestic demands develop wear-resistant corrosion resistance more Good, more environment-friendly Screwthrad sealing fat material.
The content of the invention
To solve above technical problem, the present invention provides wear-resisting environment-friendly type stop-leak compound of antirust and preparation method thereof, to solve It certainly ensure that stop-leak compound had not both contained the heavy metals such as zinc, also can guarantee that the long-term outdoor placement pipe thread non-corrosive of sleeve pipe, and The problem of remaining in that lubricity and antistick characteristic under the high temperature conditions.
The technical solution adopted by the present invention is as follows:A kind of wear-resisting environment-friendly type stop-leak compound of antirust, key is by following matter Measure the raw material composition of number:45-65 parts of universal lithium base grease, 8-20 parts of tackifier, 3-8 parts of corrosion inhibiter, complex calcium phosphate 2- 10 parts, environmentally friendly 10-18 parts of expanded graphite, 6-15 parts of polytetrafluoroethylene (PTFE).
It is preferred that, the mass fraction of the raw material is:It is 48 parts of universal lithium base grease, 9 parts of tackifier, 4 parts of corrosion inhibiter, multiple 5 parts of alloy/calcium orthophosphate, environmentally friendly 12 parts of expanded graphite, 8 parts of compositions of polytetrafluoroethylene (PTFE).
It is preferred that, the complex calcium phosphate is obtained using following methods:Calcium source is dissolved in the water respectively obtain solution A, Phosphorus source, which is dissolved in the water, obtains solution B, and the Ca/P mol ratios of the calcium source and phosphorus source are 1:(0.5-2), by solution A while stirring It is added drop-wise in solution B and obtains mixed solution;The pH value of mixed solution is remained 10~10.5 with conditioning agent, reaction is stirred at room temperature After 8-10 hours, dispersant is added, 24h is aged, by precipitation distilled water cyclic washing, in 120 DEG C of dry 2-12h;Then with 5 DEG C/min programming rates are warming up to 600 DEG C -1200 DEG C, and are incubated 0.5h-2h, that is, obtain complex calcium phosphate.
It is preferred that, the calcium source is calcium carbonate, calcium nitrate or calcium hydroxide;Phosphorus source is phosphoric acid, polyphosphoric acid or five oxygen Change two phosphorus;The conditioning agent is ammoniacal liquor or sodium hydroxide;The dispersant be triethyl group hexyl phosphoric acid, lauryl sodium sulfate or Methyl anyl alcohol.
It is preferred that, the environmentally friendly expanded graphite is obtained using following methods:Mass fraction will be sequentially added in scale graphite For 35-60% salpeter solution and oxidant, after reaction being stirred at room temperature 1-3 hours, staticly settle, sediment with distilled water repeatedly After washing, dehydrated at 120 DEG C, obtain the environmentally friendly expanded graphite.
It is preferred that, the oxidant is potassium permanganate or potassium bichromate;S contents≤50ppm of the environmentally friendly expanded graphite.
It is preferred that, the tackifier is in polybutene PB900, PB950, PB1000, PB1300, PB1400, PB2400 It is one or more.
It is preferred that, corrosion inhibiter is single pentaerythritol oleate, sorbitan monooleate, oleic acid octadecylamine or tristearin One or more in sour cyclohexylamine.
A kind of preparation method of the wear-resisting environment-friendly type stop-leak compound of antirust, key is to carry out according to the following steps:
Step 1: preparing complex calcium phosphate and environmentally friendly expanded graphite respectively;
Step 2: mix universal lithium base grease and tackifier under normal temperature, it is after being well mixed, mixture and environmental protection is swollen Swollen graphite is added in grinder, and vacuum is ground 1~10 hour, then moves into vacuum removal bubble in high-speed mixer, is obtained One mixture A;
Step 3: mixture A, corrosion inhibiter, complex calcium phosphate and polytetrafluoroethylene (PTFE) are added in high speed dispersor, vacuumize Stirring, rotating speed is 50~1000rpm, and mixing time is 70~120min, eventually passes even filter and package of mill and obtains finished product.
Beneficial effect:Compared with prior art, the wear-resisting environment-friendly type stop-leak compound of antirust of the invention introduces sustained release agent respectively And complex calcium phosphate, multiple anti-rust action is made it have, complex calcium phosphate is slightly soluble in water under corrosive environment atmosphere, to metal Chelating ability is very strong, in iron surface formation passive state envelope, with excellent rust-proof effect, environmental protection;The environmental protection expansion stone of introducing Black not sulfur-bearing (or low-sulfur), with highly expanded rate, good corrosion resistance, anti-wear performance is good;The wear-resisting environment-friendly type of antirust of the invention Stop-leak compound is different from conventional seals fat, with preferably anti-wiping property and corrosion resistance, is ensureing the premise of thread compound performance in addition Under without zinc powder, reduce risk of the heavy metal to environment, the Health cost to user reduced, with environment-friendly Property;The preparation technology of the present invention is simple, and the removal of impurity is gone using the method for fractional steps, improves dispersiveness, reduces dust pollution, environmental protection.
Embodiment
To make those skilled in the art be better understood from technical scheme, with reference to subordinate list and specific embodiment party Formula elaborates to the present invention.
First, the wear-resisting environment-friendly type stop-leak compound of a kind of antirust
Embodiment 1:The configuration proportion of each raw material in the wear-resisting environment-friendly type stop-leak compound of antirust
By each raw material in the wear-resisting environment-friendly type stop-leak compound of antirust, the mass fraction as described in table 1 is mixed respectively, obtains 3 groups The wear-resisting environment-friendly type stop-leak compound I~III of the antirust of different mixing proportion.
The wear-resisting environment-friendly type stop-leak compound of the antirust of the different mixing proportion of table 1 (mass fraction)
Embodiment 2:The preparation method of the wear-resisting environment-friendly type stop-leak compound of antirust
Step 1: the preparation of complex calcium phosphate:Dissolution of calcium carbonate is obtained into solution A, phosphoric acid in water respectively and is dissolved in water In obtain solution B, the Ca/P mol ratios of the calcium carbonate and phosphoric acid are 1:0.5, solution A is added drop-wise in solution B while stirring Obtain mixed solution;The pH value of mixed solution is remained 10~10.5 with conditioning agent, after reaction being stirred at room temperature 8-10 hours, plus Enter dispersant, 24h is aged, by precipitation distilled water cyclic washing, in 120 DEG C of dry 2-12h;Then heated up with 5 DEG C/min fast Degree is warming up to 600 DEG C -1200 DEG C, and is incubated 0.5h-2h, that is, obtains complex calcium phosphate.
The preparation of environmentally friendly expanded graphite:Will be sequentially added in scale graphite mass fraction be 35-60% salpeter solution and Potassium permanganate, after reaction being stirred at room temperature 1-3 hours, is staticly settled, and sediment is taken off with after distilled water cyclic washing at 120 DEG C Water is dried, and obtains S contents≤50ppm of the environmentally friendly expanded graphite.
Step 2: 45 parts of universal lithium base greases and 8 parts of polybutene PB900 are mixed under normal temperature, it is heated to 60~ 90 DEG C, after being well mixed, mixture and 10 parts of environmentally friendly expanded graphites are added in grinder, vacuum grinding 1~10 hour, then Vacuum removal bubble in high-speed mixer is moved into, homogeneous mixture A is obtained;
Step 3: mixture A, 3 parts of single pentaerythritol oleates, 2 parts of complex calcium phosphates and 6 parts of polytetrafluoroethylene (PTFE) are added In high speed dispersor, stirring is vacuumized, rotating speed is 50~1000rpm, and mixing time is 70~120min, eventually passes the even mistake of mill Filter is packaged to be stop-leak compound I.
Embodiment 3:The preparation method of the wear-resisting environment-friendly type stop-leak compound of antirust
Step 1: the preparation of complex calcium phosphate:Calcium nitrate is dissolved in the water respectively and obtains solution A, polyphosphoric acid and is dissolved in Solution B is obtained in water, the Ca/P mol ratios of the calcium nitrate and polyphosphoric acid are 1:2, solution A is added drop-wise to solution B while stirring In obtain mixed solution;The pH value of mixed solution is remained 10~10.5 with conditioning agent, after reaction being stirred at room temperature 8-10 hours, Dispersant is added, 24h is aged, by precipitation distilled water cyclic washing, in 120 DEG C of dry 2-12h;Then heated up with 5 DEG C/min Speed is warming up to 600 DEG C -1200 DEG C, and is incubated 0.5h-2h, that is, obtains complex calcium phosphate.
The preparation of environmentally friendly expanded graphite:Will be sequentially added in scale graphite mass fraction be 35-60% salpeter solution and Potassium bichromate, after reaction being stirred at room temperature 1-3 hours, is staticly settled, and sediment is taken off with after distilled water cyclic washing at 120 DEG C Water is dried, and obtains S contents≤20ppm of the environmentally friendly expanded graphite.
Step 2: 65 parts of universal lithium base greases and 20 parts of polybutene PB1400 are mixed under normal temperature, be heated to 60 ~90 DEG C, after being well mixed, mixture and 18 parts of environmentally friendly expanded graphites are added in grinder, vacuum grinding 1~10 hour, so Vacuum removal bubble in high-speed mixer is moved into afterwards, obtains homogeneous mixture A;
Step 3: mixture A, 8 parts of oleic acid octadecylamines, 10 parts of complex calcium phosphates and 15 parts of polytetrafluoroethylene (PTFE) are added high In fast dispersion machine, stirring is vacuumized, rotating speed is 50~1000rpm, and mixing time is 70~120min, eventually passes the even filtering of mill It is packaged to be stop-leak compound II.
Embodiment 4:The preparation method of the wear-resisting environment-friendly type stop-leak compound of antirust
Step 1: the preparation of complex calcium phosphate:Calcium hydroxide is dissolved in the water respectively and obtains solution A, phosphorus pentoxide It is dissolved in the water and obtains solution B, the Ca/P mol ratios of the calcium hydroxide and phosphorus pentoxide is 1:1, by solution A while stirring It is added drop-wise in solution B and obtains mixed solution;The pH value of mixed solution is remained 10~10.5 with conditioning agent, reaction is stirred at room temperature After 8-10 hours, dispersant is added, 24h is aged, by precipitation distilled water cyclic washing, in 120 DEG C of dry 2-12h;Then with 5 DEG C/min programming rates are warming up to 600 DEG C -1200 DEG C, and are incubated 0.5h-2h, that is, obtain complex calcium phosphate.
The preparation of environmentally friendly expanded graphite:Will be sequentially added in scale graphite mass fraction be 35-60% salpeter solution and Potassium bichromate, after reaction being stirred at room temperature 1-3 hours, is staticly settled, and sediment is taken off with after distilled water cyclic washing at 120 DEG C Water is dried, and the S contents for obtaining the environmentally friendly expanded graphite are 0.
Step 2: 48 parts of universal lithium base greases and 9 parts of polybutene PB1000 are mixed under normal temperature, it is heated to 60~ 90 DEG C, after being well mixed, mixture and 12 parts of environmentally friendly expanded graphites are added in grinder, vacuum grinding 1~10 hour, then Vacuum removal bubble in high-speed mixer is moved into, homogeneous mixture A is obtained;
Step 3: mixture A, 4 parts of sorbitan monooleates, 5 parts of complex calcium phosphates and 8 parts of polytetrafluoroethylene (PTFE) are added Enter in high speed dispersor, vacuumize stirring, rotating speed is 50~1000rpm, and mixing time is 70~120min, eventually passes mill even Filter and package and obtain stop-leak compound III.
The comparative example of embodiment 5
Equipment and operation be the same as Example 4, the difference is that complex calcium phosphate is changed into zinc powder, other raw materials and its consumption are not Become, resulting stop-leak compound IV.
The comparative example of embodiment 6
Equipment and operation be the same as Example 4, unlike environmentally friendly expanded graphite is changed to crystalline graphite powder, other raw materials and its Consumption is constant, resulting stop-leak compound V.
2nd, the stop-leak compound I~V respectively prepared the various embodiments described above requires progressive according to API RP5A3 standards It can test, it is as a result as shown in the table:
Each stop-leak compound performance test contrast table of table 2
From the data of upper table, the wear-resisting environment-friendly type stop-leak compound of antirust of the invention and the close of complex calcium phosphate is not added Lipid phase ratio is sealed, corrosion resistance is greatly improved, it is too low that stop-leak compound I-III can be seen that calcium/phosphorus mol ratio, can cause contracting The stripping quantity for closing phosphate ion is superfluous, causes stop-leak compound bulging, and rust-proof effect reduction, calcium/phosphorus mol ratio is too high, blunt due to being formed The stripping quantity of condensed phosphoric acid ion needed for state film is too low, rust-proof effect reduction;Stop-leak compound III is used compared with stop-leak compound IV Zinc powder is still not so good as the effect of complex calcium phosphate as antirust agent in terms of salt fog resistance and humidity resistance;Stop-leak compound III and sealing Fat V is compared, and due to environmentally friendly expanded graphite low-sulfur (not even sulfur-bearing), thus stability and decay resistance are more excellent.
Finally it is to be appreciated that foregoing description is only the preferred embodiments of the present invention, those skilled in the art is in the present invention Enlightenment under, on the premise of without prejudice to present inventive concept and claim, expression as multiple types can be made, it is such to become Change and each fall within protection scope of the present invention.

Claims (9)

1. the wear-resisting environment-friendly type stop-leak compound of a kind of antirust, it is characterised in that be made up of the raw material of following mass fraction:Universal lithium base 45-65 parts of lubricating grease, 8-20 parts of tackifier, 3-8 parts of corrosion inhibiter, 2-10 parts of complex calcium phosphate, environmentally friendly 10-18 parts of expanded graphite, 6-15 parts of polytetrafluoroethylene (PTFE).
2. the wear-resisting environment-friendly type stop-leak compound of antirust according to claim 1, it is characterised in that the mass fraction of the raw material For:48 parts of universal lithium base grease, 9 parts of tackifier, 4 parts of corrosion inhibiter, 5 parts of complex calcium phosphate, environmentally friendly 12 parts of expanded graphite, poly- four 8 parts of compositions of PVF.
3. the wear-resisting environment-friendly type stop-leak compound of antirust according to claim 1, it is characterised in that:The complex calcium phosphate is used Following methods are obtained:Calcium source is dissolved in the water and obtains solution A, phosphorus source, which is dissolved in the water, obtains solution B, the calcium source and phosphorus source Ca/P mol ratios be 1:(0.5-2), solution A is added drop-wise in solution B while stirring and obtains mixed solution;Will be mixed with conditioning agent The pH value for closing solution remains 10~10.5, after reaction being stirred at room temperature 8-10 hours, adds dispersant, is aged 24h, and precipitation is used Distilled water cyclic washing, in 120 DEG C of dry 2-12h;Then 600 DEG C -1200 DEG C are warming up to 5 DEG C/min programming rates, and protected Warm 0.5h-2h, that is, obtain complex calcium phosphate.
4. the wear-resisting environment-friendly type stop-leak compound of antirust according to claim 1, it is characterised in that:The calcium source be calcium carbonate, Calcium nitrate or calcium hydroxide;Phosphorus source is phosphoric acid, polyphosphoric acid or phosphorus pentoxide;The conditioning agent is ammoniacal liquor or hydroxide Sodium;The dispersant is triethyl group hexyl phosphoric acid, lauryl sodium sulfate or methyl anyl alcohol.
5. the wear-resisting environment-friendly type stop-leak compound of antirust according to claim 1, it is characterised in that:The environmentally friendly expanded graphite is adopted Obtain using the following method:The salpeter solution and oxidant that mass fraction is 35-60% will be sequentially added in scale graphite, room temperature is stirred After mixing reaction 1-3 hours, staticly settle, sediment is dehydrated with after distilled water cyclic washing at 120 DEG C, obtain described Environmentally friendly expanded graphite.
6. the wear-resisting environment-friendly type stop-leak compound of antirust according to claim 1, it is characterised in that:The oxidant is permanganic acid Potassium or potassium bichromate;S contents≤50ppm of the environmentally friendly expanded graphite.
7. the wear-resisting environment-friendly type stop-leak compound of antirust according to claim, 2,3 or 4, it is characterised in that:The tackifier are One or more in polybutene PB900, PB950, PB1000, PB1300, PB1400, PB2400.
8. the wear-resisting environment-friendly type stop-leak compound of antirust according to claim, 2,3 or 4, it is characterised in that:Corrosion inhibiter is single oil One or more in sour pentaerythritol ester, sorbitan monooleate, oleic acid octadecylamine or stearic acid cyclohexylamine.
9. the preparation method of the wear-resisting environment-friendly type stop-leak compound of antirust according to claim any one of 1-8, it is characterised in that Carry out according to the following steps:
Step 1: preparing complex calcium phosphate and environmentally friendly expanded graphite respectively;
Step 2: universal lithium base grease and tackifier are mixed under normal temperature, after being well mixed, by mixture and environmental protection expansion stone Ink is added in grinder, and vacuum is ground 1~10 hour, then moves into vacuum removal bubble in high-speed mixer, obtains homogeneous mixed Compound A;
Step 3: mixture A, corrosion inhibiter, complex calcium phosphate and polytetrafluoroethylene (PTFE) are added in high speed dispersor, vacuumize and stir Mix, rotating speed is 50~1000rpm, mixing time is 70~120min, eventually pass even filter and package of mill and obtain finished product.
CN201710397106.3A 2017-05-31 2017-05-31 Wear-resisting environment-friendly type stop-leak compound of antirust and preparation method thereof Withdrawn CN107129857A (en)

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Application publication date: 20170905