CN110128476A - A kind of phenoxy group ring phosphonitrile and its application - Google Patents
A kind of phenoxy group ring phosphonitrile and its application Download PDFInfo
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- CN110128476A CN110128476A CN201910487950.4A CN201910487950A CN110128476A CN 110128476 A CN110128476 A CN 110128476A CN 201910487950 A CN201910487950 A CN 201910487950A CN 110128476 A CN110128476 A CN 110128476A
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- Prior art keywords
- phenoxy group
- group ring
- ring phosphonitrile
- sodium
- phenol
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- ZSTLPJLUQNQBDQ-UHFFFAOYSA-N azanylidyne(dihydroxy)-$l^{5}-phosphane Chemical compound OP(O)#N ZSTLPJLUQNQBDQ-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 title claims abstract description 61
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims abstract description 62
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims abstract description 31
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 150000003388 sodium compounds Chemical class 0.000 claims abstract description 22
- 239000000047 product Substances 0.000 claims abstract description 17
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 16
- 239000011734 sodium Substances 0.000 claims abstract description 16
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 16
- 239000000706 filtrate Substances 0.000 claims abstract description 12
- 239000013078 crystal Substances 0.000 claims abstract description 10
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000013049 sediment Substances 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- 239000000463 material Substances 0.000 claims description 36
- 238000001035 drying Methods 0.000 claims description 15
- 238000005470 impregnation Methods 0.000 claims description 15
- 239000011261 inert gas Substances 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 230000002708 enhancing effect Effects 0.000 claims description 6
- 239000011888 foil Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052743 krypton Inorganic materials 0.000 claims description 4
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052754 neon Inorganic materials 0.000 claims description 4
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 4
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 2
- 238000002390 rotary evaporation Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- -1 at least one prepreg Chemical compound 0.000 description 3
- 239000012779 reinforcing material Substances 0.000 description 3
- 238000005336 cracking Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- YAVVGPBYBUYPSR-UHFFFAOYSA-N benzene;oxygen Chemical compound [O].C1=CC=CC=C1 YAVVGPBYBUYPSR-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000002650 laminated plastic Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- PQFIORQRZQVKAT-UHFFFAOYSA-N oxolane;phenol Chemical compound C1CCOC1.OC1=CC=CC=C1 PQFIORQRZQVKAT-UHFFFAOYSA-N 0.000 description 1
- FTDXCHCAMNRNNY-UHFFFAOYSA-N phenol Chemical compound OC1=CC=CC=C1.OC1=CC=CC=C1 FTDXCHCAMNRNNY-UHFFFAOYSA-N 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/6564—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms
- C07F9/6581—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms having phosphorus and nitrogen atoms with or without oxygen or sulfur atoms, as ring hetero atoms
- C07F9/65812—Cyclic phosphazenes [P=N-]n, n>=3
- C07F9/65815—Cyclic phosphazenes [P=N-]n, n>=3 n = 3
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/02—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding
- H05K3/022—Processes for manufacturing precursors of printed circuits, i.e. copper-clad substrates
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
Abstract
The invention discloses a kind of phenoxy group ring phosphonitrile and its applications, are related to phenoxy group ring phosphonitrile field.The phenoxy group ring phosphonitrile, synthesis step are as follows: first tetrahydrofuran and sodium compound are put into reaction kettle and stirred, then the tetrahydrofuran solution constant pressure containing phenol is added in reaction kettle, until the complete end of reaction of sodium compound, the tetrahydrofuran solution containing hexachlorocyclotriph,sphazene is added in reaction kettle later, it stands after sodium sediment to be chlorinated is not further added by and filters again, and filtrate is passed into Rotary Evaporators and is concentrated, then concentration filtrate is passed through and is stood in kettle, and pure water is added into standing kettle simultaneously, crystal to be precipitated is not further added by, filtering removal crystal, obtain finished product.Advantage is: simplifying phenoxy group ring phosphonitrile production stage, finished product collection rate is effectively increased, wherein collection rate is up to 98%, and purity is even more to reach 100%, the quality for additionally effectively increasing the laminate being made of phenoxy group ring phosphonitrile, has a vast market foreground.
Description
Technical field
The present invention relates to phenoxy group ring phosphonitrile technical field more particularly to a kind of phenoxy group ring phosphonitrile and its applications.
Background technique
Laminated product can be processed into various insulation and structural elements, be widely used in motor, transformer, height piezoelectricity
In device, electrical instrument and electronic equipment.Laminated product can be plate, pipe, stick or other shapes.With the development of electrical industry,
High-insulativity.High-intensitive, high temperature resistant and the laminated plastics for adapting to various use environments occur in succession.Printed circuit covers
Copper-clad laminate is also due to electronics industry needs to rapidly develop.China electrician and electronics are after liberation gradually to send out with laminated product
What exhibition was got up.China's thermosetting laminate has been formed than more completely series.The performance of laminated product depends on substrate and glues
Mixture and moulding process.Following two can be divided by its composition, characteristic and heat resistance, laminated product: (1) organic group sheet material layers
Compacting product --- with wood pulp insulating paper, coton paper, cotton etc. for reinforcing material.Long-term use temperature also develops up to 120 DEG C
Synthetic fibers products is reinforcing material；(2) inorganic substrate laminated product --- it is fine with inorganic glass fiber cloth, alkali-free glass
Tieing up felt etc. is reinforcing material.Long-term use temperature is 130 ~ 180 DEG C, and even up to higher temperature is different with binder resin.
The quality problems of laminate are resin, gluing, the concentrated expression for suppressing each process quality problems, although compacting is layer
Last one of critical process of pressing plate manufacture, but the quality of the semi-finished product of preceding processes production, will to the quality of laminate
Direct influence can be generated, therefore to the quality problems that laminate occurs, it is necessary to carry out specific analysis comprehensively, can find really
The reason of cutting adopts an effective measure solve in time, improves the quality of laminate.The current most common problem is as follows: surface
Air marks；Uneven surface, have it is stupefied；Laminate cracking；Surface middle part color depth, surrounding are whitened；Surface pressure break；Surface gum deposit；Laminate
Thickness deviation is big；Plate skids off；Dead burning plate or surface oil bloom；It is excessive to be laminated slab warping；Proof voltage is unqualified.Thus, it could be seen that electric
Requirement of the road laminate to prepreg is higher and higher, and phenoxy group ring phosphonitrile is the main material in prepreg, natural to benzene oxygen
The requirement of basic ring phosphonitrile is also higher and higher.
Summary of the invention
How the technical problem to be solved by the present invention is to solve the common quality problems of circuit laminates.
In order to solve the above technical problems, being not only simplified the present invention provides a kind of phenoxy group ring phosphonitrile and its application
Phenoxy group ring phosphonitrile production stage improves finished product collection rate, also effectively increases the laminate being made of phenoxy group ring phosphonitrile
Quality.
A kind of phenoxy group ring phosphonitrile, which is characterized in that synthesis step are as follows: under the protection of inert gas, first by tetrahydro
Furans and sodium compound are put into reaction kettle, are kept for 25~30 DEG C of temperature, are slowly stirred 1.5~3h, will then contain phenol
Tetrahydrofuran solution constant pressure is at the uniform velocity added in reaction kettle, and continues the stirring that remains a constant speed, until sodium compound has reacted completely
Finish, continue to be stirred to react 1~2.5h later and obtain phenol and receive solution, phenol is then received into solution and is heated to 65~70 DEG C, and is protected
Constant temperature is held, the tetrahydrofuran solution constant pressure containing hexachlorocyclotriph,sphazene is at the uniform velocity added in reaction kettle, and keep constant temperature, is stirred
25~30h is reacted, stands 15~20h again later, sodium sediment to be chlorinated filters after not being further added by, and filtrate is passed into rotation
It is concentrated in evaporimeter, then concentration filtrate is passed through and is stood in kettle, and pure water is added into standing kettle simultaneously, later room temperature
20~35h is stood, crystal to be precipitated is not further added by, and filtering removal crystal obtains phenoxy group ring phosphonitrile finished product.
Further, the inert gas is one of helium, neon, argon gas, Krypton and xenon.
Further, the sodium compound be sodium hydroxide or sodium, the sodium hydroxide be 40% sodium hydroxide solution,
The sodium is metallic sodium.
Further, the mass ratio of the tetrahydrofuran and sodium compound is 9:1~10:1.
Further, the content of phenol is 35~38 Kg/L in the tetrahydrofuran solution of the phenol.
Further, the purity of the hexachlorocyclotriph,sphazene is 97%, and the mass ratio of phenol and hexachlorocyclotriph,sphazene is 6:
1~7.2:1.
Further, the content of hexachlorocyclotriph,sphazene is 15~19 in the tetrahydrofuran solution of the hexachlorocyclotriph,sphazene
Kg/L。
A kind of prepreg of the phenoxy group ring phosphonitrile, it is characterised in that: the prepreg include enhancing base-material and
Pass through the phenoxy group ring phosphonitrile being attached on the enhancing base-material after impregnation drying.
The laminate of a kind of phenoxy group ring phosphonitrile, it is characterised in that: as claimed in claim 8 including at least one
Prepreg, each prepreg includes base-material and the phenoxy group ring phosphonitrile by being attached on base-material after impregnation drying.
The laminate for printed circuits of a kind of phenoxy group ring phosphonitrile, it is characterised in that: including at least two by upper
The prepreg successively overlapped under, the upper and lower surface of the prepreg are fitted with metal foil, the prepreg include base-material with
And the phenoxy group ring phosphonitrile by being attached to after impregnation drying on base-material.
Compared with prior art, it the beneficial effects of the present invention are: simplifying phenoxy group ring phosphonitrile production stage, effectively improves
Finished product collection rate, wherein collection rate is up to 98%, and purity is even more to reach 100%, is additionally effectively increased by phenoxy group ring
Phosphonitrile constitute laminate quality, reduce laminate surface air marks injustice, cracking, pressure break, surface gum deposit, thickness deviation greatly,
Plate skids off, surface oil bloom, warpage are excessive and the probabilities of occurrence such as proof voltage is unqualified, has a vast market foreground.
Specific embodiment
With reference to embodiment, the present invention is furture elucidated, it should be understood that following specific embodiments are only used for
It is bright the present invention rather than limit the scope of the invention.
Embodiment 1
A kind of phenoxy group ring phosphonitrile, synthesis step are as follows: under the protection of inert gas, first put tetrahydrofuran and sodium compound
Enter in reaction kettle, is kept for 30 DEG C of temperature, be slowly stirred 1.5h, then the tetrahydrofuran solution constant pressure containing phenol is at the uniform velocity added
Into reaction kettle, and continue the stirring that remains a constant speed, until the complete end of reaction of sodium compound, continues to be stirred to react 2.5h obtaining later
Solution is received to phenol, and phenol is then received into solution and is heated to 65 DEG C, and keeps constant temperature, by the tetrahydro furan containing hexachlorocyclotriph,sphazene
Solution constant pressure of muttering at the uniform velocity is added in reaction kettle, and keeps constant temperature, is stirred to react 30h, stands 15h again later, and sodium to be chlorinated is heavy
Starch filters after not being further added by, and filtrate is passed into Rotary Evaporators and is concentrated, and concentration filtrate is then passed through standing
In kettle, and pure water is added into standing kettle simultaneously, room temperature stands 35h later, and crystal to be precipitated is not further added by, and filtering removal is brilliant
Body obtains phenoxy group ring phosphonitrile finished product.
In the present embodiment, inert gas is one of helium, neon, argon gas, Krypton and xenon, wherein preferred
For helium, neon etc. is also can be selected in those skilled in the art.
In the present embodiment, sodium compound is sodium hydroxide, and sodium hydroxide is 40% sodium hydroxide solution, tetrahydro furan
Muttering with the mass ratio of sodium compound is 9:1, and the content of phenol is 38 Kg/L in the tetrahydrofuran solution of phenol.
In the present embodiment, the purity of hexachlorocyclotriph,sphazene is 97%, and the mass ratio of phenol and hexachlorocyclotriph,sphazene is 6:
1。
In the present embodiment, the content of hexachlorocyclotriph,sphazene is 19 Kg/L in the tetrahydrofuran solution of hexachlorocyclotriph,sphazene.
A kind of prepreg of phenoxy group ring phosphonitrile, prepreg include enhancing base-material and by being attached to this after impregnation drying
Enhance the phenoxy group ring phosphonitrile on base-material.
A kind of laminate of phenoxy group ring phosphonitrile, including at least one prepreg, each prepreg include base-material and lead to
The phenoxy group ring phosphonitrile being attached on base-material is crossed after impregnation drying.
A kind of laminate for printed circuits of phenoxy group ring phosphonitrile, the preimpregnation from top to bottom successively overlapped including at least two
Material, the upper and lower surface of prepreg are fitted with metal foil, and prepreg includes base-material and by being attached to base-material after impregnation drying
On phenoxy group ring phosphonitrile.
Embodiment 2
A kind of phenoxy group ring phosphonitrile, synthesis step are as follows: under the protection of inert gas, first put tetrahydrofuran and sodium compound
Enter in reaction kettle, is kept for 25 DEG C of temperature, be slowly stirred 3h, be then at the uniform velocity added to the tetrahydrofuran solution constant pressure containing phenol
In reaction kettle, and continue the stirring that remains a constant speed, until the complete end of reaction of sodium compound, continues to be stirred to react 1h obtaining benzene later
Phenol receives solution, and phenol is then received solution and is heated to 70 DEG C, and keeps constant temperature, and the tetrahydrofuran containing hexachlorocyclotriph,sphazene is molten
Liquid constant-pressure is at the uniform velocity added in reaction kettle, and keeps constant temperature, is stirred to react 25h, stands 20h, sodium sediment to be chlorinated again later
It is filtered after not being further added by, and filtrate is passed into Rotary Evaporators and is concentrated, then concentration filtrate is passed through and is stood in kettle,
And pure water is added into standing kettle simultaneously, room temperature stands 20h later, and crystal to be precipitated is not further added by, and filtering removal crystal obtains
To phenoxy group ring phosphonitrile finished product.
In the present embodiment, inert gas is argon gas.
In the present embodiment, it is metallic sodium that sodium compound, which is sodium hydroxide,.
In the present embodiment, the mass ratio of tetrahydrofuran and sodium compound is 10:1, benzene in the tetrahydrofuran solution of phenol
The content of phenol is 35 Kg/L, and the purity of hexachlorocyclotriph,sphazene is 97%, and the mass ratio of phenol and hexachlorocyclotriph,sphazene is 7.2:
1, the content of hexachlorocyclotriph,sphazene is 15 Kg/L in the tetrahydrofuran solution of hexachlorocyclotriph,sphazene.
A kind of prepreg of phenoxy group ring phosphonitrile, prepreg include enhancing base-material and by being attached to this after impregnation drying
Enhance the phenoxy group ring phosphonitrile on base-material.
A kind of laminate of phenoxy group ring phosphonitrile, including at least one prepreg, each prepreg include base-material and lead to
The phenoxy group ring phosphonitrile being attached on base-material is crossed after impregnation drying.
A kind of laminate for printed circuits of phenoxy group ring phosphonitrile, the preimpregnation from top to bottom successively overlapped including at least two
Material, the upper and lower surface of prepreg are fitted with metal foil, and prepreg includes base-material and by being attached to base-material after impregnation drying
On phenoxy group ring phosphonitrile.
Embodiment 3
A kind of phenoxy group ring phosphonitrile, synthesis step are as follows: under the protection of inert gas, first put tetrahydrofuran and sodium compound
Enter in reaction kettle, is kept for 28 DEG C of temperature, be slowly stirred 2.2h, then the tetrahydrofuran solution constant pressure containing phenol is at the uniform velocity added
Into reaction kettle, and continue the stirring that remains a constant speed, until the complete end of reaction of sodium compound, continues to be stirred to react 1.5h obtaining later
Solution is received to phenol, and phenol is then received into solution and is heated to 69 DEG C, and keeps constant temperature, by the tetrahydro furan containing hexachlorocyclotriph,sphazene
Solution constant pressure of muttering at the uniform velocity is added in reaction kettle, and keeps constant temperature, is stirred to react 27, stands 17h, sodium precipitating to be chlorinated again later
Object filters after not being further added by, and filtrate is passed into Rotary Evaporators and is concentrated, and concentration filtrate is then passed through standing kettle
It is interior, and pure water is added into standing kettle simultaneously, room temperature stands 30h later, and crystal to be precipitated is not further added by, and filtering removal is brilliant
Body obtains phenoxy group ring phosphonitrile finished product.
In the present embodiment, inert gas is Krypton.
In the present embodiment, sodium compound is sodium hydroxide or sodium, and the sodium hydroxide solution that sodium hydroxide is 40%, sodium is
The mass ratio of metallic sodium, tetrahydrofuran and sodium compound is 9.5:1.
In the present embodiment, in the tetrahydrofuran solution of phenol phenol content be 37 Kg/L, the four of hexachlorocyclotriph,sphazene
The content of hexachlorocyclotriph,sphazene is 17 Kg/L in hydrogen tetrahydrofuran solution.
In the present embodiment, the purity of hexachlorocyclotriph,sphazene is 97%, and the mass ratio of phenol and hexachlorocyclotriph,sphazene is
6.5:1。
A kind of prepreg of phenoxy group ring phosphonitrile, prepreg include enhancing base-material and by being attached to this after impregnation drying
Enhance the phenoxy group ring phosphonitrile on base-material.
A kind of laminate of phenoxy group ring phosphonitrile, including at least one prepreg, each prepreg include base-material and lead to
The phenoxy group ring phosphonitrile being attached on base-material is crossed after impregnation drying.
A kind of laminate for printed circuits of phenoxy group ring phosphonitrile, the preimpregnation from top to bottom successively overlapped including at least two
Material, the upper and lower surface of prepreg are fitted with metal foil, and prepreg includes base-material and by being attached to base-material after impregnation drying
On phenoxy group ring phosphonitrile.
In addition to the implementation, the present invention can also have other embodiments.It is all to use equivalent substitution or equivalent transformation shape
At technical solution, fall within the scope of protection required by the present invention.
Claims (10)
1. a kind of phenoxy group ring phosphonitrile, which is characterized in that synthesis step are as follows: under the protection of inert gas, first by tetrahydro furan
It mutters and is put into reaction kettle with sodium compound, kept for 25~30 DEG C of temperature, 1.5~3h is slowly stirred, then by four containing phenol
Hydrogen tetrahydrofuran solution constant pressure is at the uniform velocity added in reaction kettle, and continues the stirring that remains a constant speed, until the complete end of reaction of sodium compound,
Continue to be stirred to react 1~2.5h later and obtain phenol and receive solution, phenol is then received into solution and is heated to 65~70 DEG C, and keeps permanent
Tetrahydrofuran solution constant pressure containing hexachlorocyclotriph,sphazene is at the uniform velocity added in reaction kettle, and keeps constant temperature by temperature, is stirred to react
25~30h stands 15~20h again later, and sodium sediment to be chlorinated filters after not being further added by, and filtrate is passed into rotary evaporation
It is concentrated in instrument, then concentration filtrate is passed through and is stood in kettle, and pure water is added into standing kettle simultaneously, room temperature is stood later
20~35h, crystal to be precipitated are not further added by, and filtering removal crystal obtains phenoxy group ring phosphonitrile finished product.
2. a kind of phenoxy group ring phosphonitrile according to claim 1, it is characterised in that: the inert gas be helium, neon,
One of argon gas, Krypton and xenon.
3. a kind of phenoxy group ring phosphonitrile according to claim 1, it is characterised in that: the sodium compound be sodium hydroxide or
Sodium, the sodium hydroxide solution that the sodium hydroxide is 40%, the sodium are metallic sodium.
4. a kind of phenoxy group ring phosphonitrile according to claim 3, it is characterised in that: the tetrahydrofuran and sodium compound
Mass ratio is 9:1~10:1.
5. a kind of phenoxy group ring phosphonitrile according to claim 1, it is characterised in that: in the tetrahydrofuran solution of the phenol
The content of phenol is 35~38 Kg/L.
6. a kind of phenoxy group ring phosphonitrile according to claim 1, it is characterised in that: the purity of the hexachlorocyclotriph,sphazene is
97%, and the mass ratio of phenol and hexachlorocyclotriph,sphazene is 6:1~7.2:1.
7. a kind of phenoxy group ring phosphonitrile according to claim 6, it is characterised in that: the tetrahydro furan of the hexachlorocyclotriph,sphazene
The content of hexachlorocyclotriph,sphazene in solution of muttering is 15~19 Kg/L.
8. a kind of a kind of prepreg of phenoxy group ring phosphonitrile described in claim 1, it is characterised in that: the prepreg includes increasing
Strong basis material and the phenoxy group ring phosphonitrile by being attached to after impregnation drying on the enhancing base-material.
9. a kind of a kind of laminate of phenoxy group ring phosphonitrile described in claim 1, it is characterised in that: including at least one as weighed
Benefit require 8 described in prepreg, each prepreg includes base-material and the phenoxy group by being attached on base-material after impregnation drying
Ring phosphonitrile.
10. a kind of a kind of laminate for printed circuits of phenoxy group ring phosphonitrile described in claim 1, it is characterised in that: including
At least two prepregs from top to bottom successively overlapped, the upper and lower surface of the prepreg are fitted with metal foil, the preimpregnation
Material includes base-material and the phenoxy group ring phosphonitrile by being attached on base-material after impregnation drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910487950.4A CN110128476A (en) | 2019-06-05 | 2019-06-05 | A kind of phenoxy group ring phosphonitrile and its application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910487950.4A CN110128476A (en) | 2019-06-05 | 2019-06-05 | A kind of phenoxy group ring phosphonitrile and its application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110128476A true CN110128476A (en) | 2019-08-16 |
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Application publication date: 20190816 |