CN107556703A - A kind of alpha ray shield and high-voltage isulation resin combination and preparation method and application - Google Patents
A kind of alpha ray shield and high-voltage isulation resin combination and preparation method and application Download PDFInfo
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- CN107556703A CN107556703A CN201710933884.XA CN201710933884A CN107556703A CN 107556703 A CN107556703 A CN 107556703A CN 201710933884 A CN201710933884 A CN 201710933884A CN 107556703 A CN107556703 A CN 107556703A
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- resin
- lead metal
- alpha ray
- resin combination
- ray shield
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2234—Oxides; Hydroxides of metals of lead
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a kind of alpha ray shield and high-voltage isulation resin combination and preparation method and application, containing particle diameter distribution in 16 μm of ＞ in the composition epoxy resin, 10 16 μm, 10 μm of ＜ lead metal oxide powder and particle diameter distribution is at 0.5 1.0 μm, 5 μm 15 μm, lead metal powder between 1.0 5u μ ms, each powder can form equally distributed structure in resin, avoid due to agglomeration caused by skewness and particle diameter inequality, finally reduce resin internal porosity, obtain more highdensity resin material, composite is in dielectric strength, alpha ray shield effect etc. is obviously improved, in x-ray source, the field such as alpha ray shield and high-voltage isulation device has broad application prospects.
Description
Technical field
The present invention relates to alpha ray shield and high-voltage isulation resin material technical field, specially a kind of alpha ray shield and high pressure
Insualtion resin composition and preparation method and application.
Background technology
X-ray is widely used in safety check, industrial detection, medical treatment etc. perspective field, and x-ray is mainly accelerated using high pressure
Electronic impact metallic target afterwards produces, and the device that x-ray occurs is x-ray source, and x-ray source includes：X-ray generator, high pressure
Power supply unit, insulation fuel tank, control unit etc..X-ray generator includes radome and ray tube, and radome is by x-ray tube bag
Wrap up in, ray exit window and electrode extraction channel are reserved on radome, x-ray generator and high voltage supply unit etc., which are installed on, to be filled
Inside the fuel tank shell completely to insulate, radome can realize that x-ray is emitted from window at exit window, is carried out at non-exit window
Ray separates, and needs high pressure resistant breakdown between each pole of radome loading high pressure.
Technically realize radome function using pure lead, metal, leaded resin etc. at present：
(1) pure lead is used, pure lead and metal, can guarantee that excellent ray cut-off, but due to the characteristic of metallic conduction, make
Spacing increase between pole must be realized, in design by increasing the spatial volume of radome to carry with when pure lead and metal
High high-voltage isulation, so by cause x penetrate source it is heavy and difficult in maintenance etc. the problems such as；
(2) in order to avoid pure lead the problem of, domestic and international relevant unit and producer, in design using containing lead-filled epoxy resin etc.
Shielding can be solved while improve high-voltage isulation characteristic by carrying out radome design so that design to penetrate volume source small, it is in light weight,
And safety requirements can be met.
The problem of technically leaded resin is present at present：
(1) temperature characterisitic is poor, and due to formula, process variations, during product use, during special temperature rise, resin holds
Easily softening, cause the intensity decreases of product during use, the cracked failure of product etc.；
(2) insulating properties is bad, due to formula, process variations, easily goes out filler sedimentation and reunites, cause product using
Cheng Yi is in reunion point discharge breakdown；
(3) shielding properties is bad, and due to formula, process variations, product difficulty reaches high fill level, causes effective lead equivalent
Deficiency, so as to shielding properties deficiency；
(4) life-span, due to formula variation, process variations, immersion, irradiation between product is long-term in insulating oil, occur peeling,
Falling particle causes product failure.
The content of the invention
In order to solve the problems, such as that existing leaded resin material is present, the technical solution adopted by the present invention is as follows：
A kind of alpha ray shield and high-voltage isulation resin combination, it is characterised in that the resin combination is by following components group
Into：
At least two epoxy resin compositions；
At least one active epoxy diluent；
At least three kinds of polynary amine curing agent mixtures；
At least two auxiliary agents；
At least one lead metal oxide powder；
Lead metal powder；
The percentage by weight of described lead metal oxide powder is 80-90wt%, by the μ of 50-56wt%D50 particle diameters ＜ 10
M lead metal oxide, 16 μm of the lead metal oxide and 5-6wt%D50 particle diameters ＞ that 25-28wt%D50 particle diameters are 10-16 μm
Lead metal oxide composition；
The percentage by weight of described lead metal powder is 0.1-2wt%, is 0.5-1.0 μ by 0.05-1wt%D50 particle diameters
M lead metal, the lead metal that 0.03-0.6wt%D50 particle diameters are 1.0-5u μm and 0.02-0.4wt%D50 particle diameters are in 5 μm of -15 μ
M lead metal composition.
The percentage by weight of described epoxy resin composition is 10-20wt%, by bisphenol A epoxide resin, Bisphenol F epoxy
Two or more composition in resin, novolac epoxy resin or aliphatic epoxy resin, preferably bisphenol A epoxide resin and double
The mixture of phenol F epoxy resin composition.
Described composition epoxy resin is preferably by 3-16wt% bisphenol A epoxide resins and 2-10wt% Bisphenol F epoxy trees
The mixture of fat composition.
Described active epoxy diluent is AGE, butyl glycidyl ether, one kind or one kind in benzyl glycidyl ether
More than, its percentage by weight is 2.5-7wt%.
Described polynary amine curing agent mixture is diethylenetriamine, polyethylene polyamine, N- aminoethyl piperazines, epoxy change
Property IPD in three kinds or more composition, its percentage by weight is 2.1-3.0wt%.
Described polynary amine curing agent mixture is preferably by 48-65wt% diethylenetriamines, 4-12wt%N- aminoethyls
The mixture of the proportioning composition of piperazine, 3-9wt% polyethylene polyamines and the epoxide modified IPDs of 14-45wt%.
Described auxiliary agent is two kinds in polyamine acid amides dipersant, acidic polyester dipersant, organic silicon defoamer
Or two or more compositions, the wherein dosage of dispersant is the 0.1-1.5% of lead metal oxide and lead powder gross weight, defoamer
Dosage is the 0.1-2% of epoxy resin composition gross weight.
Described lead metal oxide is the one or more in PbO, Pb3O4, PbO2.
A kind of described alpha ray shield and the preparation method of high-voltage isulation resin combination, it is characterised in that step is as follows：
Step 1, epoxy resin is weighed in proportion, be mixed evenly；
Step 2, weigh in proportion in the component that active epoxy diluent is added obtained by step 1, add to stirring while stirring
Uniformly；
Step 3, weigh in the blending ingredients that dispersant is added obtained by step 2, be uniformly mixed in proportion；
Step 4, weigh in the component that lead metal oxide component is added obtained by step 3, add when scattered, extremely in proportion
It is uniformly dispersed at a high speed；
Step 5, weigh in the component that lead metal powder is added obtained by step 4, disperse when adding in proportion, it is scattered to high speed
Uniformly；
Step 6, weigh in the component that organic silicon defoamer is added obtained by step 5, be uniformly mixed in proportion；
Step 7, polynary amine curing agent component is weighed in proportion, be well mixed；
Step 8, the component obtained by the curing agent component and step 6 that are mixed in step 7 is mixed evenly in proportion；
Step 9, the component vacuumizing and defoaming that completion will be well mixed in step 8, it is processed good to be poured into after completion deaeration
Cavity or mould in, stand 2-24h after insert in baking oven, under the conditions of 50~70 DEG C solidify 120~150min, solidified
It is stripped, produces after complete.
The present invention also protects application of the described resin combination in x-ray source, alpha ray shield and high-voltage isulation device.
Compared with prior art, the lead oxides containing the distribution of three class different grain sizes in composition epoxy resin of the invention
Powder and the lead metal powder of three class different grain sizes distribution, wherein lead metal oxide powder particle size are distributed in 16 μm of ＞, 10-16
μm, between 10 μm of ＜, lead metal powder size overcomes simple between 5 μm -15 μm, 0.5-1.0 μm, 1.0-5u μ ms
The defects of leaded resin high-pressure poor insulativity, the alpha ray shield performance of lead oxides modified resin is improved, simultaneously because lead is golden
Each powder of category powder and lead metal oxide powder can form equally distributed structure in resin, avoid due to skewness
With agglomeration caused by particle diameter inequality, finally reduce resin internal porosity, obtain more highdensity resin material, it is compound
Material is obviously improved in dielectric strength, alpha ray shield effect etc., exhausted in x-ray source, alpha ray shield and high pressure
The fields such as edge device have broad application prospects.
Embodiment
Technical solution of the present invention is described further below by embodiment.
The raw material and equipment used in embodiment：
Raw material：Electron level pellet powder PbO, Pb3O4、PbO2, micro/nano level Pb powder, commercially available bisphenol A epoxide resin, commercially available Bisphenol F
Epoxy resin, commercially available novolac epoxy resin, AGE, diethylenetriamine, polyethylene polyamine, N- aminoethyl piperazines, epoxide modified different Buddhist
That ketone diamines, acidic polyester solution, organic silicon defoamer；
Equipment：Dispersion machine, particle size analyzer, viscosimeter, hardometer, omnipotent push-and-pull machine, high-tension resistive tester, conductometer.
Embodiment 1-27
Embodiment 1-27 resin combination is prepared according to following steps according to each component of the formula ratio of table 2：
Step 1, resin premixed material prepared according to table 1；
Step 2, weigh in the resin premixed material that dispersant is added obtained by step 1, be uniformly mixed in proportion；
Step 3, the particle diameter for determining with particle size analyzer lead metal oxide, weigh according to the ratio of table 1 and match, obtain lead oxides
Premix, then adds this premix in the component obtained by step 3, adds when scattered, to being uniformly dispersed at a high speed；
Step 4, lead metal powder footpath is determined with particle size analyzer, and weigh proportioning in proportion, gained lead metal powder adds step 3
In the component of gained, disperse when adding, to being uniformly dispersed at a high speed；
Step 5, weigh in the component that organic silicon defoamer is added obtained by step 4, be uniformly mixed in proportion；
Step 6, polynary amine curing agent component weighed according to the ratio of table 1, be well mixed, obtain curing agent premix；
Component obtained by step 7, the curing agent premix by step 6 and step 6 is mixed evenly in proportion；
Step 8, the component vacuumizing and defoaming that completion will be well mixed in step 7, it is processed good to be poured into after completion deaeration
Cavity or mould in, stand 2-24h after insert in baking oven, under the conditions of 50~70 DEG C solidify 120~150min, solidified
It is stripped after complete, obtains alpha ray shield and high-voltage isulation Resin Composition Example 1-27.The premix that embodiment 1-27 is used is matched somebody with somebody
Measure and its see Tables 1 and 2 with the formula ratio of other components in side；The performance of resin combination obtained by embodiment 1-27 is shown in Table 3.
The embodiment 1-27 premix formulations of table 1
The formula of each resin combinations of embodiment 1-27 of table 2
The embodiment 1-27 resin combination physical performances of table 3
Claims (10)
1. a kind of alpha ray shield and high-voltage isulation resin combination, it is characterised in that the resin combination is composed of the following components：
At least two epoxy resin compositions；
At least one active epoxy diluent；
At least three kinds of polynary amine curing agent mixtures；
At least two auxiliary agents；
At least one lead metal oxide powder；
Lead metal powder；
The percentage by weight of described lead metal oxide powder is 80-90 wt%, by 10 μm of 50-56 wt%D50 particle diameters ＜'s
16 μm of the lead metal oxide and 5-6 wt%D50 particle diameters ＞ that lead metal oxide, 25-28 wt%D50 particle diameters are 10-16 μm
Lead metal oxide forms；
The percentage by weight of described lead metal powder is 0.1-2 wt%, is 0.5-1.0 μm by 0.05-1 wt%D50 particle diameters
Lead metal, the lead metal that 0.03-0.6 wt%D50 particle diameters are 1.0-5u μm and 0.02-0.4 wt%D50 particle diameters are at 5 μm -15 μm
Lead metal forms.
2. a kind of alpha ray shield as claimed in claim 1 and high-voltage isulation resin combination, it is characterised in that described epoxy
The percentage by weight of resin compound is 10-20 wt%, by bisphenol A epoxide resin, bisphenol F epoxy resin, novolac epoxy resin
Or two or more composition in aliphatic epoxy resin, preferably bisphenol A epoxide resin and bisphenol F epoxy resin form
Mixture.
3. a kind of alpha ray shield as claimed in claim 1 and high-voltage isulation resin combination, it is characterised in that described epoxy
The mixture that resin combination is preferably made up of 3-16wt% bisphenol A epoxide resins and 2-10wt% bisphenol F epoxy resins.
4. a kind of alpha ray shield as claimed in claim 1 and high-voltage isulation resin combination, it is characterised in that described activity
Epoxide diluent is AGE, the one or more in butyl glycidyl ether, benzyl glycidyl ether, its percentage by weight
For 2.5-7 wt%.
5. a kind of alpha ray shield as claimed in claim 1 and high-voltage isulation resin combination, it is characterised in that described is polynary
Amine-type cure agent composition is in diethylenetriamine, polyethylene polyamine, N- aminoethyl piperazines, epoxide modified IPD
Three kinds or more forms, and its percentage by weight is 2.1-3.0 wt%.
6. a kind of alpha ray shield as claimed in claim 1 and high-voltage isulation resin combination, it is characterised in that described is polynary
Preferably by 48-65 wt% diethylenetriamines, 4-12 wt%N- aminopiperazines, 3-9 wt%, more ethene is more for amine-type cure agent composition
The mixture of the proportioning composition of amine and the epoxide modified IPDs of 14-45 wt%.
7. a kind of alpha ray shield as claimed in claim 1 and high-voltage isulation resin combination, it is characterised in that described auxiliary agent
For in polyamine acid amides dipersant, acidic polyester dipersant, organic silicon defoamer two or more composition, wherein
The dosage of dispersant is lead metal oxide and the 0.1-1.5% of lead powder gross weight, and the dosage of defoamer is epoxy resin composition
The 0.1-2% of gross weight.
8. a kind of alpha ray shield as claimed in claim 1 and high-voltage isulation resin combination, it is characterised in that described lead gold
It is PbO, Pb to belong to oxide3O4、PbO2In one or more.
9. the preparation method of a kind of alpha ray shield as claimed in claim 1 and high-voltage isulation resin combination, it is characterised in that
Step is as follows：
Step 1, epoxy resin is weighed in proportion, be mixed evenly；
Step 2, weigh in proportion in the component that active epoxy diluent is added obtained by step 1, add to stir while stirring；
Step 3, weigh in the blending ingredients that dispersant is added obtained by step 2, be uniformly mixed in proportion；
Step 4, weigh in the component that lead metal oxide component is added obtained by step 3, add when scattered, to high speed in proportion
It is uniformly dispersed；
Step 5, weigh in the component that lead metal powder is added obtained by step 4, disperse when adding in proportion, it is scattered equal to high speed
It is even；
Step 6, weigh in the component that organic silicon defoamer is added obtained by step 5, be uniformly mixed in proportion；
Step 7, polynary amine curing agent component is weighed in proportion, be well mixed；
Step 8, the component obtained by the curing agent component and step 6 that are mixed in step 7 is mixed evenly in proportion；
Step 9, the component vacuumizing and defoaming that completion will be well mixed in step 8, processed good chamber is poured into after completing deaeration
In body or mould, inserted after standing 2-24h in baking oven, solidify 120 ~ 150min under the conditions of 50 ~ 70 DEG C, taken off after completion of cure
Mould, produce.
10. the resin combination as described in claim 1-8 is any is in x-ray source, alpha ray shield and high-voltage isulation device
Using.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210823846.XA CN115058097A (en) | 2017-10-10 | 2017-10-10 | Ray shielding and high-voltage insulating resin composition and preparation method and application thereof |
| CN201710933884.XA CN107556703A (en) | 2017-10-10 | 2017-10-10 | A kind of alpha ray shield and high-voltage isulation resin combination and preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710933884.XA CN107556703A (en) | 2017-10-10 | 2017-10-10 | A kind of alpha ray shield and high-voltage isulation resin combination and preparation method and application |
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| CN202210823846.XA Division CN115058097A (en) | 2017-10-10 | 2017-10-10 | Ray shielding and high-voltage insulating resin composition and preparation method and application thereof |
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| CN107556703A true CN107556703A (en) | 2018-01-09 |
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| CN202210823846.XA Pending CN115058097A (en) | 2017-10-10 | 2017-10-10 | Ray shielding and high-voltage insulating resin composition and preparation method and application thereof |
| CN201710933884.XA Pending CN107556703A (en) | 2017-10-10 | 2017-10-10 | A kind of alpha ray shield and high-voltage isulation resin combination and preparation method and application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276646A (en) * | 2018-02-06 | 2018-07-13 | 中国船舶重工集团公司第七〇九研究所 | A kind of proportioning type composite shielding material and preparation method thereof with neutron and the comprehensive shielded effects of γ |
| CN109401206A (en) * | 2018-12-24 | 2019-03-01 | 张冬生 | A kind of Epocryl base shielding material |
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| CN102595754A (en) * | 2012-01-06 | 2012-07-18 | 同方威视技术股份有限公司 | Radiation device installing box and oil cooling cyclic system as well as X-ray generator |
| CN106867201A (en) * | 2017-03-06 | 2017-06-20 | 苏州镭瑞机电科技有限公司 | A kind of part lead semi-annular jade pendant and manufacture method for High-Voltage Insulation and alpha ray shield |
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| CA2231008A1 (en) * | 1997-03-05 | 1998-09-05 | Thin Film Technology, Inc. | Polymeric composition for radiation shielding |
| KR101297099B1 (en) * | 2011-05-13 | 2013-08-20 | 한국원자력연구원 | Epoxy resin compositions for neutron shielding materials and mehtod for preparing the same |
| CN104710727B (en) * | 2015-03-27 | 2017-11-17 | 中国科学院长春应用化学研究所 | Epoxy resin-matrix neutron and gamma ray shielding composite and preparation method and application |
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2017
- 2017-10-10 CN CN202210823846.XA patent/CN115058097A/en active Pending
- 2017-10-10 CN CN201710933884.XA patent/CN107556703A/en active Pending
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| CN102595754A (en) * | 2012-01-06 | 2012-07-18 | 同方威视技术股份有限公司 | Radiation device installing box and oil cooling cyclic system as well as X-ray generator |
| CN106867201A (en) * | 2017-03-06 | 2017-06-20 | 苏州镭瑞机电科技有限公司 | A kind of part lead semi-annular jade pendant and manufacture method for High-Voltage Insulation and alpha ray shield |
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| 马延洪: "《X线物理与防护》", 30 April 1990, 人民卫生出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276646A (en) * | 2018-02-06 | 2018-07-13 | 中国船舶重工集团公司第七〇九研究所 | A kind of proportioning type composite shielding material and preparation method thereof with neutron and the comprehensive shielded effects of γ |
| CN109401206A (en) * | 2018-12-24 | 2019-03-01 | 张冬生 | A kind of Epocryl base shielding material |
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| CN115058097A (en) | 2022-09-16 |
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Application publication date: 20180109 |