CN109048122A - A kind of preparation method of the disposable flux material of high activity - Google Patents
A kind of preparation method of the disposable flux material of high activity Download PDFInfo
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- CN109048122A CN109048122A CN201810943379.8A CN201810943379A CN109048122A CN 109048122 A CN109048122 A CN 109048122A CN 201810943379 A CN201810943379 A CN 201810943379A CN 109048122 A CN109048122 A CN 109048122A
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- parts
- disposable
- high activity
- acid
- flux material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/362—Selection of compositions of fluxes
Abstract
The present invention relates to a kind of preparation methods of the disposable flux material of high activity, belong to flux material technical field.Technical solution of the present invention is compound using the phytic acid and chlorogenic acid extracted and to film forming agent poly-vinyl alcohol solution modification, since with the hydroxyl on polyvinyl alcohol esterification can occur in a heated condition for the phosphate radical on phytic acid, to make poly-vinyl alcohol solution macromolecular crosslink, film forming agent after being crosslinked simultaneously has excellent mechanical property and intensity, the phytic acid and chlorogenic acid Compound-acid that technical solution of the present invention uses simultaneously are modified material, pass through phytic acid, chlorogenic acid and tartaric acid compounding, keep the boiling point of these activating agents stepped, keep scaling powder that can play activity in each temperature range, simultaneously, compound the acidic activator formed, the acid intensity of material is effectively reduced, while reduction to material surface corrosive nature, reduce the viscosity that activator uses rear material, lacking for impurity is adhered to after further decreasing material activation It falls into.
Description
Technical field
The present invention relates to a kind of preparation methods of the disposable flux material of high activity, belong to flux material technical field.
Background technique
In welding, the oxide layer that metal surface is formed can interfere welding effect, usually use certain particular matters to remove
These oxides are removed, to reach good welds.This energy purification is waved metal surface, the substance welded is helped to call helping by people
Solder flux.Scaling powder is indispensable material in electronics assembly technology, by physics and chemical influence welding process, most
End form is at reliable bright spot.Helping and selecting agent is a kind of mixture with multiple action, being capable of direct shadow in Electronic Assemblies technique
The q&r for ringing product, is to help most important auxiliary material in wlding material.The fast development of modern electronics industry and
The raising that precise electronic degree requires, the effect and requirement to scaling powder are also higher and higher.Currently, constantly changing with lead-free solder
Into development, researchers at home and abroad pair matched with brightness material use help brightness agent to carry out a large amount of research.From traditional colophony type
Scaling powder sets out, and the change of component and the control of content are carried out to it, tries hard to develop a kind of pair of environment and human body pollution-free, nontoxic
Harmful inexpensive scaling powder, experienced following several stages: the scaling powder of colophony type containing halogen, halogen-free colophony type scaling powder and nothing
Halogen is without colophony type scaling powder.
Currently, the research emphasis of lead-free solder scaling powder is no-clean scaling powder, Halogen is this without no-clean scaling powder
One kind of class scaling powder, because it has without rosin, halogen-free, solid content is low, nonflammable, convenient storage, will not pollute ring
The advantages that border will not be detrimental to health, free of cleaning increasingly causes to pay close attention to and pay attention to.But lead-free solder is universal at present with scaling powder
There is a problem of the weaker, moistening badness of activity, more than residual, and a large amount of pollution environment can be generated in the welding process and endanger people
The organic matter of body health.Therefore, the vital task that Halogen is field without no-clean scaling powder is developed.It is welded using lead-free solder
When, the excessively high effective component volatilization for being easy to cause scaling powder of welding temperature is too fast, and guidance causes the failure of scaling powder performance, loses
Activation and protective effect, to be easy to produce the defects of waving ball and bridging；But some activators can only be dissolved in traditional alcohols object
Thus the range of choice of activator is very limited matter, and the selection of each component is also highly difficult, and other compositions are exempted from low-solid content
Cleaning scaling powder is identical, including activator, surfactant etc., these are usually no more than at total amount is got, in addition it is also possible to consider
The agent of additive amount wetting agent come increase solder flux wetability thus improve material welding activity performance it is necessary.
Summary of the invention
The technical problems to be solved by the invention: for existing flux material welding activity it is bad, be also easy to produce wave ball and
The problem of the defects of bridging, provides a kind of preparation method of disposable flux material of high activity.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) honeysuckle is mixed with perilla leaf and vacuum freeze drying and is ground, collects abrasive flour and mistake by 1:5 in mass ratio
Sieve collects sieving powder；
(2) sieving powder is stirred with ethanol solution, collects mixed liquor juxtaposition and impregnate at room temperature by 1:10 in mass ratio,
Ultrasound assisted extraction again is collected extracting solution and is filtered, collects to obtain filtrate；
(3) 1:5 in mass ratio, by filtrate added drop-wise into poly-vinyl alcohol solution, after being added dropwise to complete, Heat preservation reaction is collected
Mixed liquor is placed in rotary evaporation, obtains revolving liquid；
(4) according to parts by weight, 45~50 parts of deionized waters, 1~2 part of tartaric acid, 3~5 parts of OP-10,3~5 parts are weighed respectively
5% diethylene glycol ether of mass fraction, 3~5 parts of 5% nitroethanes of mass fraction, 0.1~0.5 part of benzotriazole and 15~
20 parts of revolving liquid are placed in three-necked flask, insulation reaction, and standing is cooled to room temperature and collects to obtain reaction solution, are centrifugated and are collected
Supernatant liquor can be prepared into the disposable flux material of high activity.
Abrasive flour described in step (1) is 80 mesh abrasive flours.
Filtrate added drop-wise rate described in step (3) is 2~3mL/min.
Rotating evaporation temperature described in step (3) is 45~55 DEG C.
Centrifuge separation rate described in step (3) is 1500~2000r/min.
The present invention is compared with other methods, and advantageous effects are:
Technical solution of the present invention is compound using the phytic acid and chlorogenic acid extracted and to film forming agent poly-vinyl alcohol solution modification, by
Esterification can occur in a heated condition with the hydroxyl on polyvinyl alcohol in the phosphate radical on phytic acid, to make polyvinyl alcohol
Solution macromolecular crosslinks, while the film forming agent after crosslinking has excellent mechanical property and intensity, while the technology of the present invention
The phytic acid and chlorogenic acid Compound-acid that scheme uses are modified material, are compounded by phytic acid, chlorogenic acid and tartaric acid, make these
The boiling point of activating agent is stepped, keeps scaling powder that can play activity in each temperature range, meanwhile, compound the acidity of formation
The acid intensity of material is effectively reduced in activator, while reduction to material surface corrosive nature, reduces activator and uses rear material
The viscosity of material further decreases the defect of adherency impurity after material activation.
Specific embodiment
Honeysuckle is mixed with perilla leaf and vacuum freeze drying and is ground, collects abrasive flour and mistake by 1:5 in mass ratio
80 meshes collect sieving powder and 1:10 in mass ratio, and sieving powder is stirred with 80% ethanol solution of mass fraction, is received
Collection mixed liquor juxtaposition impregnates 10~12h, then 3~5h of ultrasound assisted extraction at 45~55 DEG C, 200~300W at room temperature, receives
Collection extracting solution simultaneously filters, and collects to obtain filtrate；1:5 in mass ratio, by filtrate added drop-wise into 8% poly-vinyl alcohol solution of mass fraction,
Control drop rate is 2~3mL/min, and Heat preservation reacts 3~5h after being added dropwise to complete, then at 65~70 DEG C, is collected mixed
Conjunction liquid is placed in rotation at 45~55 DEG C and is evaporated to the 1/5 of mixeding liquid volume, obtains revolving liquid；According to parts by weight, it weighs respectively
45~50 parts of deionized waters, 1~2 part of tartaric acid, 3~5 parts of OP-10,3~5 parts of 5% diethylene glycol ethers of mass fraction, 3~5
5% nitroethane of part mass fraction, 0.1~0.5 part of benzotriazole and 15~20 parts of revolving liquid are placed in three-necked flask, by three
Mouth flask is placed in 2~3h of insulation reaction at 75~80 DEG C, and standing is cooled to room temperature and collects to obtain reaction solution, places reaction liquid into
Supernatant liquor is centrifugated and collected under 1500~2000r/min, can be prepared into the disposable flux material of high activity.
Honeysuckle is mixed with perilla leaf and vacuum freeze drying and is ground, collects abrasive flour and mistake by 1:5 in mass ratio
80 meshes collect sieving powder and 1:10 in mass ratio, and sieving powder is stirred with 80% ethanol solution of mass fraction, is received
Collection mixed liquor juxtaposition impregnates 10h, then the ultrasound assisted extraction 3h at 45 DEG C, 200W at room temperature, collects extracting solution and filters, receives
Collect to obtain filtrate；1:5 in mass ratio, by filtrate added drop-wise into 8% poly-vinyl alcohol solution of mass fraction, control drop rate is 2mL/
Min, Heat preservation reacts 3h after being added dropwise to complete, then at 65 DEG C, collect mixed liquor be placed at 45 DEG C rotation be evaporated to it is mixed
The 1/5 of liquid product is closed, revolving liquid is obtained；According to parts by weight, 45 parts of deionized waters, 1 part of tartaric acid, 3 parts of OP-10,3 are weighed respectively
5% diethylene glycol ether of part mass fraction, 3 parts of 5% nitroethanes of mass fraction, 0.1 part of benzotriazole and 15 parts of revolving liquid
It is placed in three-necked flask, three-necked flask is placed in insulation reaction 2h at 75 DEG C, standing is cooled to room temperature and collects to obtain reaction solution, will
Reaction solution, which is placed under 1500r/min, is centrifugated and collects supernatant liquor, can be prepared into the high activity cleaning-free scaling powder
Material.
Honeysuckle is mixed with perilla leaf and vacuum freeze drying and is ground, collects abrasive flour and mistake by 1:5 in mass ratio
80 meshes collect sieving powder and 1:10 in mass ratio, and sieving powder is stirred with 80% ethanol solution of mass fraction, is received
Collection mixed liquor juxtaposition impregnates 11h, then the ultrasound assisted extraction 4h at 47 DEG C, 250W at room temperature, collects extracting solution and filters, receives
Collect to obtain filtrate；1:5 in mass ratio, by filtrate added drop-wise into 8% poly-vinyl alcohol solution of mass fraction, control drop rate is 2mL/
Min, Heat preservation reacts 4h after being added dropwise to complete, then at 67 DEG C, collect mixed liquor be placed at 47 DEG C rotation be evaporated to it is mixed
The 1/5 of liquid product is closed, revolving liquid is obtained；According to parts by weight, 47 parts of deionized waters, 2 parts of tartaric acid, 4 parts of OP-10,4 are weighed respectively
5% diethylene glycol ether of part mass fraction, 4 parts of 5% nitroethanes of mass fraction, 0.2 part of benzotriazole and 17 parts of revolving liquid
It is placed in three-necked flask, three-necked flask is placed in insulation reaction 2h at 77 DEG C, standing is cooled to room temperature and collects to obtain reaction solution, will
Reaction solution, which is placed under 1750r/min, is centrifugated and collects supernatant liquor, can be prepared into the high activity cleaning-free scaling powder
Material.
Honeysuckle is mixed with perilla leaf and vacuum freeze drying and is ground, collects abrasive flour and mistake by 1:5 in mass ratio
80 meshes collect sieving powder and 1:10 in mass ratio, and sieving powder is stirred with 80% ethanol solution of mass fraction, is received
Collection mixed liquor juxtaposition impregnates 12h, then the ultrasound assisted extraction 5h at 55 DEG C, 300W at room temperature, collects extracting solution and filters, receives
Collect to obtain filtrate；1:5 in mass ratio, by filtrate added drop-wise into 8% poly-vinyl alcohol solution of mass fraction, control drop rate is 3mL/
Min, Heat preservation reacts 5h after being added dropwise to complete, then at 70 DEG C, collect mixed liquor be placed at 55 DEG C rotation be evaporated to it is mixed
The 1/5 of liquid product is closed, revolving liquid is obtained；According to parts by weight, 50 parts of deionized waters, 2 parts of tartaric acid, 5 parts of OP-10,5 are weighed respectively
5% diethylene glycol ether of part mass fraction, 5 parts of 5% nitroethanes of mass fraction, 0.5 part of benzotriazole and 20 parts of revolving liquid
It is placed in three-necked flask, three-necked flask is placed in insulation reaction 3h at 80 DEG C, standing is cooled to room temperature and collects to obtain reaction solution, will
Reaction solution, which is placed under 2000r/min, is centrifugated and collects supernatant liquor, can be prepared into the high activity cleaning-free scaling powder
Material.
Example 1,2,3 prepared by the present invention is tested for the property, specific test result is as follows shown in table table 1:
1 performance test table of table
As seen from the above table, there is scaling powder prepared by the present invention excellent helping to weld effect and activity.
Claims (5)
1. a kind of preparation method of the disposable flux material of high activity, it is characterised in that specific preparation step are as follows:
(1) honeysuckle is mixed with perilla leaf and vacuum freeze drying and is ground, collects abrasive flour and mistake by 1:5 in mass ratio
Sieve collects sieving powder；
(2) sieving powder is stirred with ethanol solution, collects mixed liquor juxtaposition and impregnate at room temperature by 1:10 in mass ratio,
Ultrasound assisted extraction again is collected extracting solution and is filtered, collects to obtain filtrate；
(3) 1:5 in mass ratio, by filtrate added drop-wise into poly-vinyl alcohol solution, after being added dropwise to complete, Heat preservation reaction is collected
Mixed liquor is placed in rotary evaporation, obtains revolving liquid；
(4) according to parts by weight, 45~50 parts of deionized waters, 1~2 part of tartaric acid, 3~5 parts of OP-10,3~5 parts are weighed respectively
5% diethylene glycol ether of mass fraction, 3~5 parts of 5% nitroethanes of mass fraction, 0.1~0.5 part of benzotriazole and 15~
20 parts of revolving liquid are placed in three-necked flask, insulation reaction, and standing is cooled to room temperature and collects to obtain reaction solution, are centrifugated and are collected
Supernatant liquor can be prepared into the disposable flux material of high activity.
2. a kind of preparation method of the disposable flux material of high activity according to claim 1, it is characterised in that: step
(1) abrasive flour described in is 80 mesh abrasive flours.
3. a kind of preparation method of the disposable flux material of high activity according to claim 1, it is characterised in that: step
(3) the filtrate added drop-wise rate described in is 2~3mL/min.
4. a kind of preparation method of the disposable flux material of high activity according to claim 1, it is characterised in that: step
(3) rotating evaporation temperature described in is 45~55 DEG C.
5. a kind of preparation method of the disposable flux material of high activity according to claim 1, it is characterised in that: step
(3) the centrifuge separation rate described in is 1500~2000r/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810943379.8A CN109048122A (en) | 2018-08-17 | 2018-08-17 | A kind of preparation method of the disposable flux material of high activity |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810943379.8A CN109048122A (en) | 2018-08-17 | 2018-08-17 | A kind of preparation method of the disposable flux material of high activity |
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| CN109048122A true CN109048122A (en) | 2018-12-21 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201810943379.8A Withdrawn CN109048122A (en) | 2018-08-17 | 2018-08-17 | A kind of preparation method of the disposable flux material of high activity |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110964134A (en) * | 2019-12-11 | 2020-04-07 | 哈尔滨工程大学 | Preparation method of polyvinyl alcohol phytate |
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| CN1565791A (en) * | 2003-07-03 | 2005-01-19 | 梁树华 | Wash-free film forming water-based type welding flux |
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| CN102699576A (en) * | 2012-04-18 | 2012-10-03 | 广东工业大学 | Low-VOC (volatile organic compound) non-cleaning flux comprising complex surfactant and method for preparing same |
| CN103756599A (en) * | 2013-12-24 | 2014-04-30 | 上海邦中高分子材料有限公司 | Adhesive resin with high temperature resistance and high adhesive strength |
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| CN101104231A (en) * | 2007-08-11 | 2008-01-16 | 厦门大学 | Cleaning-free water base type scaling powder capable of restraining welding point interface compound growth |
| CN102398124A (en) * | 2011-04-12 | 2012-04-04 | 广东工业大学 | Water-based cleaning-free flux for lead-free welding flux and preparation method thereof |
| CN102699576A (en) * | 2012-04-18 | 2012-10-03 | 广东工业大学 | Low-VOC (volatile organic compound) non-cleaning flux comprising complex surfactant and method for preparing same |
| CN103756599A (en) * | 2013-12-24 | 2014-04-30 | 上海邦中高分子材料有限公司 | Adhesive resin with high temperature resistance and high adhesive strength |
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Non-Patent Citations (1)
| Title |
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| 宋德花等: "正交试验法优选金银花中绿原酸超声波强化浸出工艺研究", 《中兽医医药杂志》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110964134A (en) * | 2019-12-11 | 2020-04-07 | 哈尔滨工程大学 | Preparation method of polyvinyl alcohol phytate |
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Application publication date: 20181221 |
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