CN102636511A - Test method of optimal cross-linking agent diffusion time in production process of high-voltage cable material - Google Patents

Test method of optimal cross-linking agent diffusion time in production process of high-voltage cable material Download PDF

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CN102636511A
CN102636511A CN2012101549680A CN201210154968A CN102636511A CN 102636511 A CN102636511 A CN 102636511A CN 2012101549680 A CN2012101549680 A CN 2012101549680A CN 201210154968 A CN201210154968 A CN 201210154968A CN 102636511 A CN102636511 A CN 102636511A
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crosslinking chemical
diffusion time
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hydrogen atom
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CN102636511B (en
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韩宝忠
赵洪
李长明
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Harbin University of Science and Technology
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Abstract

The invention discloses a test method of optimal cross-linking agent diffusion time in the production process of a high-voltage cable material, relates to a test method of a cross-linking agent diffusion time in the production process of the high-voltage cable material. The method can be used for solving the problem that the optimal cross-linking agent diffusion time in the production process of the cross-linkable high-voltage cable material is hard to determine. The method comprises the following steps: in the production process, sampling 1 g of m from particles at intervals of 0.5 hour, placing the material in absolute ethyl alcohol to stand at a constant temperature, filtering, and then collecting the filtrate; adding a chloroform solution of ethyl p-hydroxybenzoate in a nuclear magnetic tube, volatilizing the chloroform, adding the filtrate in the nuclear magnetic tube, and adding a deuterated chloroform, uniformly mixing, testing a H spectrum of the to-be-tested solution in the test tube in the step sixth, computing the concentration difference of the cross-linking agent at the particle centre at two adjacent sampling times, and determining the optimal cross-linking agent diffusion time. The method provided by the invention has the advantages of high tested data precision, small experimental amount, shortened test time and low cost. The method is used for testing the optimal cross-linking agent diffusion time in the production process of the high-voltage cable material.

Description

The method of testing of best crosslinking chemical diffusion time in the high-tension cable manufacture of materials process
Technical field
The present invention relates to the method for testing of diffusion time of crosslinking chemical in the high-tension cable manufacture of materials process.
Background technology
Along with social progress and rapid economy development, powerful to the demand growth of electric energy in the world wide, consumption is anxious in recent years increases for the carrier that power cable transports as electric energy.Advantages such as dielectric properties are good because of having for cross-linked polyethylene insulated cable, transmission capacity is big, laying installation and operation maintenance are convenient, the trend that substitutes other kind cable in recent years is obvious further, the consumption cumulative year after year.Especially in the high-tension cable field, 110kV and above electric pressure high-pressure cross-linking cable mainly adopt crosslinked polyetylene insulated, and 500kV level ultra-high voltage cross-linking polyethylene insulated cable also is applied in the line.This situation has also promoted domestic quick increase to crosslinkable high-tension cable materials demand.Crosslinkable high-voltage cable insulating material and semiconductive shieldin material are mainly produced by Dow Chemical company, company of Borealis and Korea S Han Hua company in the world at present; Wherein Dow Chemical company and company of Borealis have occupied most markets of 110kV and above electric pressure crosslinkable cable material, the whole dependence on import of the present required crosslinkable high-tension cable material of China.
Under state-of-the art, peroxide crosslinking technology is the unique channel of producing high-pressure cross-linking cable.Because high-voltage cable insulating internal electric field intensity is higher, if having impurity than large scale, gel etc., can cause that then the regional area electric field further concentrates, become the root that electric branch causes, finally cause cable life to reduce even the insulation rapid damage.Therefore, the size of impurity, gel and quantity must strictly control in the high-voltage cable insulating, and requirement does not contain above impurity of 100 μ m and the above gel of 200 μ m usually.The ultrapure clean production technology of cable material is the major technique bottleneck that restricts China's crosslinkable high-tension cable domestic material at present.The source of impurity, gel has two in the crosslinkable high-tension cable material: the one, and self contains starting material, mainly is removed through the filtering technique in producing; The 2nd, in the production run of crosslinkable high-tension cable material, newly produce, this will be avoided occurring through the production technology design.The production technology of the reasonable crosslinkable high-tension cable material of generally acknowledging at present is the back absorption process: earlier with auxiliary agent melt blending, filtration, granulation, dryings such as tygon and antioxidant; Physical mixed is evenly and store certain hour under a certain constant temperature with this granular scavenging material and liquid crosslinking chemical then; Make crosslinking chemical be diffused into the center gradually, finally reach even distribution from the particulate material surface.In storage temperature one regularly, crosslinking chemical diffusion profile homogeneity depends on the constant temperature storage time: if the constant temperature storage time is short, then crosslinking chemical skewness in particulate material finally causes the manufacturing cable performance not meet the demands; If the constant temperature storage time is long, then production efficiency is low.Therefore, in crosslinkable high-tension cable manufacture of materials process, must confirm granular scavenging material and mixed best constant temperature storage time of liquid crosslinking chemical, promptly best crosslinking chemical diffusion time according to production technology.
One Chinese patent application---a kind of method of testing crosslinking chemical degree of scatter in the crosslinkable high-tension cable material; Application number is 201110272035.7; This patent discloses a kind of method of testing crosslinking chemical degree of scatter in the crosslinkable high-tension cable material, existence not enough as follows:
(1) in the application liquid chromatography test solution during concentration of crosslinking chemical, for same sample, the possibility of result that different instruments record can be different, and the possibility of result that flow rate of liquid does not record simultaneously also can be variant.Therefore, when adopting the method, must guarantee that all samples of same batch all use same liquid chromatograph to test, and all conditions in the test process is all identical.The result that different instruments, different test condition obtain does not have comparability;
(2) test result receives the influence of impurity in the crosslinking chemical easily;
(3) quantitative accuracy is not high, for confirming the optimal absorption time, needs the top layer of the same time sampling of contrast and the concentration of center crosslinking chemical, when the difference of the two is not more than 0.1%, reaches requirement, and experimental amount is big.
Summary of the invention
The present invention will solve the problem that best crosslinking chemical in the production run of crosslinkable high-tension cable material is not easy to confirm diffusion time, and the method for diffusion time of best crosslinking chemical in a kind of definite high-tension cable manufacture of materials is provided.
The method of testing of best crosslinking chemical diffusion time is carried out according to the following steps in the high-tension cable manufacture of materials process of the present invention:
One, absorption process is produced in the high-tension cable materials process after utilization; Physical mixed is evenly and store under constant temperature for the particulate material that granular scavenging material that will obtain through raw materials melt blend, filtration, granulation, drying and liquid crosslinking chemical are formed; After the storage; Every interval 0.5h takes out 30～50 gram particulate material as sample, is designated as i sample time;
The centermost of the particulate material sample that two, obtains in each sampling cuts the cube that the length of side is 0.4～0.6mm, and this cubical quality is designated as m 1Gram, m 1=0.2～1.0 grams;
Three, the m that step 2 is cut 1Gram material and m 2The gram absolute ethyl alcohol is put into test tube and sealing, test tube is put into 60～70 ℃ constant temperature water tank again, leaves standstill 5～8h, wherein m 1: m 2=1: (10～20);
Four, the solidliquid mixture in will the test tube after step 3 is handled filters, and collects the filtrating sealing and preserves, and is to be measured by sampling time i numbering;
Five, get m 3The gram ethyl-para-hydroxybenzoate with dissolved in chloroform and be settled to 5mL, obtains the chloroformic solution of ethyl-para-hydroxybenzoate, in the nuclear-magnetism pipe, adds the chloroformic solution of the above-mentioned ethyl-para-hydroxybenzoate of 0.1mL, uncoveredly then vapors away whole chloroforms; M wherein 3=0.1～0.2 gram;
Six, 0.4mL step 4 gained filtrating is joined in the nuclear-magnetism pipe that has vapored away chloroform in the step 5, add the 0.1mL deuterochloroform again, to be measured behind the mixing;
Seven, utilize the H spectrum of liquid to be measured in the nmr determination step 6 nuclear-magnetism pipe, and according to the concentration M of spectrogram by crosslinking chemical in the following formula calculation procedure four gained filtrating i:
Figure BDA00001655477400031
In the formula:
M i-step 4 gained is the concentration of crosslinking chemical in the filtrating of i corresponding to sample time, the g/mL of unit;
S 1-calculate in the nmr spectrum corresponding to the spectrum peak area of demarcating hydrogen atom on the ethyl-para-hydroxybenzoate molecule, it is decided to be 1;
S 2In-the nmr spectrum corresponding to the spectrum peak area of demarcating hydrogen atom on the cross-linker molecules with corresponding to the spectrum peak area S that demarcates hydrogen atom on the ethyl-para-hydroxybenzoate molecule 1Ratio, it is identical to demarcate on hydrogen atom and the ethyl-para-hydroxybenzoate molecule demarcation hydrogen atom present position characteristic on the cross-linker molecules;
Demarcate the number of hydrogen atom on each cross-linker molecules of n-;
Eight, calculate the particulate material sample center crosslinker concentration ω that surveys by following formula i:
ω i = M i m 2 ρ 1 m 1 ρ 2 ( ρ 1 - M i ) × 100 %
In the formula:
ω i-corresponding to the particulate material sample center crosslinker concentration that is i sample time, massfraction, %;
ρ 1-crosslinking chemical proportion, g/cm 3
ρ 2-absolute ethyl alcohol proportion, g/cm 3
Nine, by formula Calculate the particulate material sample center crosslinker concentration difference percent ω of adjacent two sample times Δ, when the concentration difference percent is no more than 2%, can confirm that (i-0.5) hour is best crosslinking chemical diffusion time.
The invention has the beneficial effects as follows: the present invention utilizes NMR to test; Test gained data precision is high; Utilize different instrument test gained results consistent, have comparability, with application number be 201110272035.7 one Chinese patent application---a kind of method of testing crosslinking chemical degree of scatter in the crosslinkable high-tension cable material is compared; Experimental amount can reduce half the, has shortened test duration and cost greatly.
The present invention is used for the diffusion time of the best crosslinking chemical of testing high voltage cable material production run.
Description of drawings
Fig. 1 be in the embodiment of the invention one when i=8 the H of liquid to be measured spectrum in the step 6 test tube;
Fig. 2 be in the embodiment of the invention one when i=8.5 the H of liquid to be measured spectrum in the step 6 test tube.
Embodiment
Technical scheme of the present invention is not limited to following cited embodiment, also comprises the combination in any between each embodiment.
Embodiment one: the method for testing of best crosslinking chemical diffusion time is carried out according to the following steps in this embodiment high-tension cable manufacture of materials process:
One, absorption process is produced in the high-tension cable materials process after utilization; Physical mixed is evenly and store under constant temperature for the particulate material that granular scavenging material that will obtain through raw materials melt blend, filtration, granulation, drying and liquid crosslinking chemical are formed; After the storage; Every interval 0.5h takes out 30～50 gram particulate material as sample, is designated as i sample time;
The centermost of the particulate material sample that two, obtains in each sampling cuts the cube that the length of side is 0.4～0.6mm, and this cubical quality is designated as m 1Gram, m 1=0.2～1.0 grams;
Three, the m that step 2 is cut 1Gram material and m 2The gram absolute ethyl alcohol is put into test tube and sealing, test tube is put into 60～70 ℃ constant temperature water tank again, leaves standstill 5～8h, wherein m 1: m 2=1: (10～20);
Four, the solidliquid mixture in will the test tube after step 3 is handled filters, and collects the filtrating sealing and preserves, and is to be measured by sampling time i numbering;
Five, get m 3The gram ethyl-para-hydroxybenzoate with dissolved in chloroform and be settled to 5mL, obtains the chloroformic solution of ethyl-para-hydroxybenzoate, in the nuclear-magnetism pipe, adds the chloroformic solution of the above-mentioned ethyl-para-hydroxybenzoate of 0.1mL, uncoveredly then vapors away whole chloroforms; M wherein 3=0.1～0.2 gram;
Six, 0.4mL step 4 gained filtrating is joined in the nuclear-magnetism pipe that has vapored away chloroform in the step 5, add the 0.1mL deuterochloroform again, to be measured behind the mixing;
Seven, utilize the H spectrum of liquid to be measured in the nmr determination step 6 nuclear-magnetism pipe, and according to the concentration M of spectrogram by crosslinking chemical in the following formula calculation procedure four gained filtrating i:
Figure BDA00001655477400041
In the formula:
M i-step 4 gained is the concentration of crosslinking chemical in the filtrating of i corresponding to sample time, the g/mL of unit;
S 1-calculate in the nmr spectrum corresponding to the spectrum peak area of demarcating hydrogen atom on the ethyl-para-hydroxybenzoate molecule, it is decided to be 1;
S 2In-the nmr spectrum corresponding to the spectrum peak area of demarcating hydrogen atom on the cross-linker molecules with corresponding to the spectrum peak area S that demarcates hydrogen atom on the ethyl-para-hydroxybenzoate molecule 1Ratio, it is identical to demarcate on hydrogen atom and the ethyl-para-hydroxybenzoate molecule demarcation hydrogen atom present position characteristic on the cross-linker molecules;
Demarcate the number of hydrogen atom on each cross-linker molecules of n-;
Eight, calculate the particulate material sample center crosslinker concentration ω that surveys by following formula i:
ω i = M i m 2 ρ 1 m 1 ρ 2 ( ρ 1 - M i ) × 100 %
In the formula:
ω i-corresponding to the particulate material sample center crosslinker concentration that is i sample time, massfraction, %;
ρ 1-crosslinking chemical proportion, g/cm 3
ρ 2-absolute ethyl alcohol proportion, g/cm 3
Nine, by formula
Figure BDA00001655477400052
Calculate the particulate material sample center crosslinker concentration difference percent ω of adjacent two sample times Δ, when the concentration difference percent is no more than 2%, can confirm that (i-0.5) hour is best crosslinking chemical diffusion time.
The beneficial effect of this embodiment is: this embodiment utilizes NMR to test; Test gained data precision is high; Utilize different instrument test gained results consistent, have comparability, with application number be 201110272035.7 one Chinese patent application---a kind of method of testing crosslinking chemical degree of scatter in the crosslinkable high-tension cable material is compared; Experimental amount can reduce half the, has shortened test duration and cost greatly.
Embodiment two: what this embodiment and embodiment one were different is: in the step 2, the centermost of the particulate material that obtains in each sampling cuts the cube that the length of side is 0.5mm.Other is identical with embodiment one.
Embodiment three: what this embodiment was different with embodiment one or two is: in the step 3, and the m that step 2 is cut 1Gram material and m 2The gram absolute ethyl alcohol is put into test tube and sealing, test tube is put into 65 ℃ constant temperature water tank again, leaves standstill 6～7h.Other is identical with embodiment one or two.
Embodiment four: what this embodiment was different with one of embodiment one to three is: in the step 3, and m 1: m 2=1: (12～18).Other is identical with one of embodiment one to three.
Embodiment five: what this embodiment was different with one of embodiment one to four is: in the step 5, and m 3=0.12～0.18 gram.Other is identical with one of embodiment one to four.
Embodiment six: what this embodiment was different with one of embodiment one to five is: in the step 7, selected demarcation hydrogen atom present position characteristic has following characteristics: (1) is positioned on the phenyl ring, links to each other with a carbon atom on the phenyl ring; (2) coupled carbon atom also with phenyl ring on 2 carbon atoms link to each other, 2 ortho position carbon atoms are promptly arranged; (3) wherein 1 ortho position carbon atom and 1 hydrogen atom link to each other with 1 carbon atom in addition on the phenyl ring; In addition 1 ortho position carbon atom links to each other with phenyl ring 1 carbon atom outward with 1 carbon atom in addition in the phenyl ring.Other is identical with one of embodiment one to five.
Adopt following examples to verify beneficial effect of the present invention:
Embodiment one: present embodiment is produced the high-tension cable cross-linkable polyethylene insulation material with cumyl peroxide (DCP) as crosslinking chemical, and the method for testing of best crosslinking chemical diffusion time is carried out according to the following steps in the high-tension cable manufacture of materials process:
One, absorption process is produced in the high-tension cable materials process after utilization; Physical mixed is evenly and store under constant temperature for the particulate material that granular scavenging material that will obtain through raw materials melt blend, filtration, granulation, drying and liquid crosslinking chemical are formed; After the storage; Every interval 0.5h takes out 30 gram particulate material as sample, is designated as i sample time;
The centermost of the particulate material sample that two, obtains in each sampling cuts the cube that the length of side is 0.4～0.6mm, and this cubical quality is designated as m 1Gram;
Three, the m that step 2 is cut 1Gram material and m 2The gram absolute ethyl alcohol is put into test tube and sealing, test tube is put into 60 ℃ constant temperature water tank again, leaves standstill 8h, wherein m 1: m 2=1: 10;
Four, the solidliquid mixture in will the test tube after step 3 is handled filters, and collects the filtrating sealing and preserves, and is to be measured by sampling time i numbering;
Five, get m 3The gram ethyl-para-hydroxybenzoate with dissolved in chloroform and be settled to 5mL, obtains the chloroformic solution of ethyl-para-hydroxybenzoate, in the nuclear-magnetism pipe, adds the chloroformic solution of the above-mentioned ethyl-para-hydroxybenzoate of 0.1mL, uncoveredly then vapors away whole chloroforms;
Six, 0.4mL step 4 gained filtrating is joined in the nuclear-magnetism pipe that has vapored away chloroform in the step 5, add the 0.1mL deuterochloroform again, to be measured behind the mixing;
Seven, utilize the H spectrum of liquid to be measured in the nmr determination step 6 test tube, and according to the concentration M of spectrogram by crosslinking chemical in the following formula calculation procedure four gained filtrating i:
Figure BDA00001655477400061
In the formula:
M i-step 4 gained is the concentration of crosslinking chemical in the filtrating of i corresponding to sample time, the g/mL of unit;
S 1-calculate in the nmr spectrum corresponding to the spectrum peak area of demarcating hydrogen atom on the ethyl-para-hydroxybenzoate molecule, it is decided to be 1, the molecular formula of ethyl-para-hydroxybenzoate of demarcating hydrogen atom in the present embodiment is following, the hydrogen atom of H for demarcating of band ☆:
Figure BDA00001655477400071
S 2In-the nmr spectrum corresponding to the spectrum peak area of demarcating hydrogen atom on the cross-linker molecules with corresponding to the spectrum peak area S that demarcates hydrogen atom on the ethyl-para-hydroxybenzoate molecule 1Ratio, demarcate on the cross-linker molecules that to demarcate hydrogen atom present position characteristic on hydrogen atom and the ethyl-para-hydroxybenzoate molecule identical, the molecular formula of crosslinking chemical of demarcating hydrogen atom in the present embodiment is following, the H of band ☆ is the hydrogen atom of demarcation:
Figure BDA00001655477400072
Demarcate the number of hydrogen atom on each cross-linker molecules of n-;
Eight, calculate the particulate material center crosslinker concentration ω that surveys by following formula i:
ω i = M i m 2 ρ 1 m 1 ρ 2 ( ρ 1 - M i ) × 100 %
In the formula:
ω i-corresponding to the particulate material center crosslinker concentration that is i sample time, massfraction, %;
ρ 1-crosslinking chemical proportion, g/cm 3
ρ 2-absolute ethyl alcohol proportion, g/cm 3
Nine, by formula
Figure BDA00001655477400074
calculates the particulate material center crosslinker concentration percentage difference of adjacent two sample times; When the concentration difference percent is no more than 2%, can confirm that (i-0.5) hour is best crosslinking chemical diffusion time.
When be 8h sample time, record data were following:
(1) i=8 in the step 1;
(2) m in the step 2 1=0.2g;
(3) m in the step 3 2=5g;
(4) m in the step 5 3=0.12639g;
(5) contain 4 among the DCP and demarcate hydrogen atom, i.e. n=4;
(6) relative molecular mass of ethyl-para-hydroxybenzoate is 166.18;
(7) relative molecular mass of DCP is 270.37;
(8) as shown in Figure 1 in the nmr spectrum corresponding to demarcating the spectrum peak of demarcating hydrogen atom on hydrogen atom and the cross-linker molecules on the ethyl-para-hydroxybenzoate molecule;
(9) get S by nmr spectrum 2=0.0700;
(10) according to the concentration M of crosslinking chemical in formula calculation procedure four gained in the step 7 filtrating 8:
M 8 = 0.12639 × 0 . 0700 × 270.37 25 × 4 × 1 × 166.17 = 1 . 44 × 10 - 4 ( mg / mL )
(11) DCP crosslinking chemical proportion ρ 1=1.082g/cm 3
(12) absolute ethyl alcohol proportion ρ 2=0.7893g/cm 3
(13) calculate the particulate material center crosslinker concentration ω that surveys according to the formula in the step 8 8:
ω 8 = 1.44 × 10 - 4 × 5 × 1.082 0.2 × 0 . 7893 ( 1.082 - 1.44 × 10 - 4 ) × 100 % = 0.456 %
When be 8.5h sample time, record data were following:
(1) i=8.5 in the step 1;
(2) m in the step 2 1=0.2g;
(3) m in the step 3 2=5g;
(4) m in the step 5 3=0.12639g;
(5) contain 4 among the DCP and demarcate hydrogen atom, i.e. n=4;
(6) relative molecular mass of ethyl-para-hydroxybenzoate is 166.18;
(7) relative molecular mass of DCP is 270.37;
(8) as shown in Figure 2 in the nmr spectrum corresponding to demarcating the spectrum peak of demarcating hydrogen atom on hydrogen atom and the cross-linker molecules on the ethyl-para-hydroxybenzoate molecule;
(9) get S by nmr spectrum 2=0.1036;
(10) according to the concentration M of crosslinking chemical in formula calculation procedure four gained in the step 7 filtrating 8.5:
M 8.5 = 0.12639 × 0.1036 × 270.37 25 × 4 × 1 × 166.17 = 2.13 × 10 - 4 ( mg / mL )
(11) DCP crosslinking chemical proportion ρ 1=1.082g/cm 3
(12) absolute ethyl alcohol proportion ρ 2=0.7893g/cm 3
(13) calculate the particulate material center crosslinker concentration ω that surveys according to the formula in the step 8 8.5:
ω 8.5 = 2.95 × 10 - 4 × 5 × 1.082 0.2 × 0.7893 × ( 1.082 - 2.95 × 10 - 4 ) × 100 % = 0.675 %
Formula in nine calculates the particulate material center crosslinker concentration difference percent of adjacent two sample times set by step:
ω 8.5 - ω 8 ω 8 × 100 % = 48.0 %
This concentration difference percent surpasses 2%, can confirm it 8 hours was not best crosslinking chemical diffusion time, needs to continue to increase crosslinking chemical diffusion time.
Present embodiment utilizes NMR to test; Test gained data precision is high; Utilize different instrument test gained results consistent, have comparability, with application number be 201110272035.7 one Chinese patent application---a kind of method of testing crosslinking chemical degree of scatter in the crosslinkable high-tension cable material is compared; Experimental amount can reduce half the, has shortened test duration and cost greatly.

Claims (6)

1. the method for testing of best crosslinking chemical diffusion time in the high-tension cable manufacture of materials process is characterized in that the method for testing of best crosslinking chemical in high-tension cable manufacture of materials process diffusion time is carried out according to the following steps:
One, absorption process is produced in the high-tension cable materials process after utilization; Physical mixed is evenly and store under constant temperature for the particulate material that granular scavenging material that will obtain through raw materials melt blend, filtration, granulation, drying and liquid crosslinking chemical are formed; After the storage; Every interval 0.5h takes out 30～50 gram particulate material as sample, is designated as i sample time;
The centermost of the particulate material sample that two, obtains in each sampling cuts the cube that the length of side is 0.4～0.6mm, and this cubical quality is designated as m 1Gram, m 1=0.2～1.0 grams;
Three, the m that step 2 is cut 1Gram material and m 2The gram absolute ethyl alcohol is put into test tube and sealing, test tube is put into 60～70 ℃ constant temperature water tank again, leaves standstill 5～8h, wherein m 1: m 2=1: (10～20);
Four, the solidliquid mixture in will the test tube after step 3 is handled filters, and collects the filtrating sealing and preserves, and is to be measured by sampling time i numbering;
Five, get m 3The gram ethyl-para-hydroxybenzoate with dissolved in chloroform and be settled to 5mL, obtains the chloroformic solution of ethyl-para-hydroxybenzoate, in the nuclear-magnetism pipe, adds the chloroformic solution of the above-mentioned ethyl-para-hydroxybenzoate of 0.1mL, uncoveredly then vapors away whole chloroforms; M wherein 3=0.1～0.2 gram;
Six, 0.4mL step 4 gained filtrating is joined in the nuclear-magnetism pipe that has vapored away chloroform in the step 5, add the 0.1mL deuterochloroform again, to be measured behind the mixing;
Seven, utilize the H spectrum of liquid to be measured in the nmr determination step 6 nuclear-magnetism pipe, and according to the concentration M of spectrogram by crosslinking chemical in the following formula calculation procedure four gained filtrating i:
Figure FDA00001655477300011
In the formula:
M i-step 4 gained is the concentration of crosslinking chemical in the filtrating of i corresponding to sample time, the g/mL of unit;
S 1-calculate in the nmr spectrum corresponding to the spectrum peak area of demarcating hydrogen atom on the ethyl-para-hydroxybenzoate molecule, it is decided to be 1;
S 2In-the nmr spectrum corresponding to the spectrum peak area of demarcating hydrogen atom on the cross-linker molecules with corresponding to the spectrum peak area S that demarcates hydrogen atom on the ethyl-para-hydroxybenzoate molecule 1Ratio, it is identical to demarcate on hydrogen atom and the ethyl-para-hydroxybenzoate molecule demarcation hydrogen atom present position characteristic on the cross-linker molecules;
Demarcate the number of hydrogen atom on each cross-linker molecules of n-;
Eight, calculate the particulate material sample center crosslinker concentration ω that surveys by following formula i:
ω i = M i m 2 ρ 1 m 1 ρ 2 ( ρ 1 - M i ) × 100 %
In the formula:
ω i-corresponding to the particulate material sample center crosslinker concentration that is i sample time, massfraction, %;
ρ 1-crosslinking chemical proportion, g/cm 3
ρ 2-absolute ethyl alcohol proportion, g/cm 3
Nine, by formula
Figure FDA00001655477300022
Calculate the particulate material sample center crosslinker concentration difference percent ω of adjacent two sample times Δ, when the concentration difference percent is no more than 2%, can confirm that (i-0.5) hour is best crosslinking chemical diffusion time.
2. the method for testing of best crosslinking chemical diffusion time is characterized in that in the step 2 in the high-tension cable manufacture of materials process according to claim 1, and the centermost of the particulate material that obtains in each sampling cuts the cube that the length of side is 0.5mm.
3. the method for testing of best crosslinking chemical diffusion time is characterized in that in the step 3 in the high-tension cable manufacture of materials process according to claim 1, the m that step 2 is cut 1Gram material and m 2The gram absolute ethyl alcohol is put into test tube and sealing, test tube is put into 65 ℃ constant temperature water tank again, leaves standstill 6～7h.
4. the method for testing of best crosslinking chemical diffusion time is characterized in that in the step 3 m in the high-tension cable manufacture of materials process according to claim 1 1: m 2=1: (12～18).
5. the method for testing of best crosslinking chemical diffusion time is characterized in that in the step 5 m in the high-tension cable manufacture of materials process according to claim 1 3=0.12～0.18 gram.
6. the method for testing of best crosslinking chemical diffusion time in the high-tension cable manufacture of materials process according to claim 1; It is characterized in that in the step 7; Selected demarcation hydrogen atom present position characteristic has following characteristics: (1) is positioned on the phenyl ring, links to each other with a carbon atom on the phenyl ring; (2) coupled carbon atom also with phenyl ring on 2 carbon atoms link to each other, 2 ortho position carbon atoms are promptly arranged; (3) wherein 1 ortho position carbon atom and 1 hydrogen atom link to each other with 1 carbon atom in addition on the phenyl ring; In addition 1 ortho position carbon atom links to each other with phenyl ring 1 carbon atom outward with 1 carbon atom in addition in the phenyl ring.
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CN106908468A (en) * 2017-03-03 2017-06-30 西安近代化学研究所 Gel state cloud detonator cross-linked state Changing Pattern detecting system under high temperature

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CN102276901A (en) * 2011-07-19 2011-12-14 哈尔滨理工大学 Method for preparing ultraclean crosslinkable polyethylene insulation material of high-voltage cable
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Publication number Priority date Publication date Assignee Title
CN106908468A (en) * 2017-03-03 2017-06-30 西安近代化学研究所 Gel state cloud detonator cross-linked state Changing Pattern detecting system under high temperature
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