CN117067334B - 一种木材表面防火防腐处理工艺 - Google Patents
一种木材表面防火防腐处理工艺 Download PDFInfo
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- CN117067334B CN117067334B CN202311351810.7A CN202311351810A CN117067334B CN 117067334 B CN117067334 B CN 117067334B CN 202311351810 A CN202311351810 A CN 202311351810A CN 117067334 B CN117067334 B CN 117067334B
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- 239000002023 wood Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 23
- 230000008569 process Effects 0.000 title claims abstract description 23
- 230000002421 anti-septic effect Effects 0.000 title claims description 11
- 238000005260 corrosion Methods 0.000 claims abstract description 78
- 238000006243 chemical reaction Methods 0.000 claims abstract description 51
- 238000010438 heat treatment Methods 0.000 claims abstract description 49
- 239000004359 castor oil Substances 0.000 claims abstract description 42
- 235000019438 castor oil Nutrition 0.000 claims abstract description 42
- 239000011248 coating agent Substances 0.000 claims abstract description 42
- 238000000576 coating method Methods 0.000 claims abstract description 42
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims abstract description 42
- WMKGGPCROCCUDY-PHEQNACWSA-N dibenzylideneacetone Chemical compound C=1C=CC=CC=1\C=C\C(=O)\C=C\C1=CC=CC=C1 WMKGGPCROCCUDY-PHEQNACWSA-N 0.000 claims abstract description 35
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000003063 flame retardant Substances 0.000 claims abstract description 33
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- 239000003431 cross linking reagent Substances 0.000 claims abstract description 29
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- 239000000178 monomer Substances 0.000 claims abstract description 28
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 25
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims abstract description 22
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- RPHKINMPYFJSCF-UHFFFAOYSA-N benzene-1,3,5-triamine Chemical compound NC1=CC(N)=CC(N)=C1 RPHKINMPYFJSCF-UHFFFAOYSA-N 0.000 claims abstract description 14
- RFSBGZWBVNPVNN-UHFFFAOYSA-N 2,4,6-tris(ethenyl)-2,4,6-trimethyl-1,3,5,2,4,6-triazatrisilinane Chemical compound C=C[Si]1(C)N[Si](C)(C=C)N[Si](C)(C=C)N1 RFSBGZWBVNPVNN-UHFFFAOYSA-N 0.000 claims abstract description 13
- UBIJTWDKTYCPMQ-UHFFFAOYSA-N hexachlorophosphazene Chemical compound ClP1(Cl)=NP(Cl)(Cl)=NP(Cl)(Cl)=N1 UBIJTWDKTYCPMQ-UHFFFAOYSA-N 0.000 claims abstract description 13
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229930040373 Paraformaldehyde Natural products 0.000 claims abstract description 12
- 229920002866 paraformaldehyde Polymers 0.000 claims abstract description 12
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000027 potassium carbonate Inorganic materials 0.000 claims abstract description 11
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- QIGBRXMKCJKVMJ-UHFFFAOYSA-N 1,4-Benzenediol Natural products OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 14
- JOXIMZWYDAKGHI-UHFFFAOYSA-N p-toluenesulfonic acid Substances CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 14
- 238000010025 steaming Methods 0.000 claims description 12
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 10
- 125000003396 thiol group Chemical group [H]S* 0.000 claims description 9
- 238000002390 rotary evaporation Methods 0.000 claims description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 6
- 239000003973 paint Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 239000003381 stabilizer Substances 0.000 claims description 4
- JRGTXQUZUGCTFP-UHFFFAOYSA-N 2-hydroxy-1,5-diphenylpenta-1,4-dien-3-one Chemical compound OC(C(C=CC1=CC=CC=C1)=O)=CC1=CC=CC=C1 JRGTXQUZUGCTFP-UHFFFAOYSA-N 0.000 claims description 2
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- 125000000687 hydroquinonyl group Chemical group C1(O)=C(C=C(O)C=C1)* 0.000 claims description 2
- 125000005489 p-toluenesulfonic acid group Chemical group 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- RGHHSNMVTDWUBI-UHFFFAOYSA-N 4-hydroxybenzaldehyde Chemical compound OC1=CC=C(C=O)C=C1 RGHHSNMVTDWUBI-UHFFFAOYSA-N 0.000 description 14
- KZMGYPLQYOPHEL-UHFFFAOYSA-N Boron trifluoride etherate Chemical compound FB(F)F.CCOCC KZMGYPLQYOPHEL-UHFFFAOYSA-N 0.000 description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 12
- 238000012360 testing method Methods 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 6
- 150000001336 alkenes Chemical group 0.000 description 6
- 238000009835 boiling Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- NIQQIJXGUZVEBB-UHFFFAOYSA-N methanol;propan-2-one Chemical compound OC.CC(C)=O NIQQIJXGUZVEBB-UHFFFAOYSA-N 0.000 description 6
- 239000003208 petroleum Substances 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- 239000000376 reactant Substances 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 6
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000007106 1,2-cycloaddition reaction Methods 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CMLFRMDBDNHMRA-UHFFFAOYSA-N 2h-1,2-benzoxazine Chemical group C1=CC=C2C=CNOC2=C1 CMLFRMDBDNHMRA-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 238000001723 curing Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
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- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000004971 Cross linker Substances 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 238000003848 UV Light-Curing Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
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- 239000003085 diluting agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- -1 hexachlorocyclo-triphosphazene nitrogen-phosphorus structure Chemical group 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
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- 230000009545 invasion Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
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- 239000003755 preservative agent Substances 0.000 description 1
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- 239000002994 raw material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
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- 230000001954 sterilising effect Effects 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D191/00—Coating compositions based on oils, fats or waxes; Coating compositions based on derivatives thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/02—Processes; Apparatus
- B27K3/12—Impregnating by coating the surface of the wood with an impregnating paste
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/16—Inorganic impregnating agents
- B27K3/18—Compounds of alkaline earth metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/34—Organic impregnating agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/34—Organic impregnating agents
- B27K3/343—Heterocyclic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/34—Organic impregnating agents
- B27K3/36—Aliphatic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/34—Organic impregnating agents
- B27K3/38—Aromatic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/34—Organic impregnating agents
- B27K3/38—Aromatic compounds
- B27K3/40—Aromatic compounds halogenated
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/52—Impregnating agents containing mixtures of inorganic and organic compounds
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
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- B27K2240/00—Purpose of the treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
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Abstract
本发明涉及中木材表面防火防腐处理技术领域,公开了一种木材表面防火防腐处理工艺,包括以下步骤:将含酚羟基二苄叉丙酮、烯丙基缩水甘油醚、咪唑和丁基羟基甲苯加热至反应,得到交联剂;将含酚羟基二苄叉丙酮、1,3,5‑三氨基苯、多聚甲醛加入二氧六环中加热反应,得到支化单体;将支化单体、六氯环三膦腈和无水碳酸钾,氮气氛围下加热反应,得到复合防腐阻燃剂:将复合防腐阻燃剂、交联剂、2,4,6‑三甲基‑2,4,6‑三乙烯基环三硅氮烷和2,2‑二羟甲基丙酸依次加入巯基改性蓖麻油中搅拌均匀,得到防火防腐涂料;将防腐防火涂料均匀涂覆在木材表面,光固化,得到表面防火防腐层。
Description
技术领域
本发明涉及木材表面防火防腐处理技术领域,具体为一种木材表面防火防腐处理工艺。
背景技术
木材作为一种天然绿色有机材料,其自身面临着在储存过程中,由于适当的水分、空气和温度的作用下,受到真菌、昆虫等侵害导致木材受损后发生腐朽变质,严重损害木材及木制品的使用寿命。同时,木材使用场景多为室内密闭,狭小空间中,在人们生活中无处不在,其自身的易燃性质也带来了许多安全隐患。
因此,发明一种木材表面防火防腐处理工艺具有重要意义
发明内容
本发明的目的在于提供一种木材表面防火防腐处理工艺,以解决上述背景技术中提出的问题。
为了解决上述技术问题,本发明提供如下技术方案:
一种木材表面防火防腐处理工艺,包含以下步骤:
S1:将含酚羟基二苄叉丙酮、1,3,5-三氨基苯、多聚甲醛加入二氧六环中,在80-85℃下反应5-6h,旋蒸,得到支化单体;将支化单体和六氯环三膦腈加入四氢呋喃中,加入无水碳酸钾,氮气氛围下加热至75-80℃反应8-9h,过滤,旋蒸,提纯,得到复合防腐阻燃剂;
S2:将复合防腐阻燃剂、交联剂、2,4,6-三甲基-2,4,6-三乙烯基环三硅氮烷和2,2-二羟甲基丙酸依次加入巯基改性蓖麻油中搅拌均匀,得到防火防腐涂料;将防腐防火涂料均匀涂覆在木材表面,光固化,得到表面防火防腐层。
进一步的,所述交联剂制备方法包括以下步骤:
将含酚羟基二苄叉丙酮、烯丙基缩水甘油醚、咪唑和丁基羟基甲苯依次加入氮气氛围反应容器中搅拌均匀,加热至100-105℃反应25-30min,继续加热至110-115℃反应3-3.5h,最后加热至122-125℃反应1-1.5h,冷却沉淀,纯化,得到交联剂。
进一步的,所述含酚羟基二苄叉丙酮:烯丙基缩水甘油醚的质量比为(5-6):(4-5);所述咪唑加入量为含酚羟基二苄叉丙酮加入量的1.8-2.5wt%;所述丁基羟基甲苯加入量为含酚羟基二苄叉丙酮加入量的0.5-0.8wt%。
进一步的,所述巯基改性蓖麻油制备方法包括以下步骤:
将蓖麻油、催化剂和稳定剂加入甲苯中搅拌均匀,氮气氛围下加热至110-115℃,加入3-巯基丙酸搅拌反应5-6h,冷却,旋蒸,得到巯基改性蓖麻油。
进一步的,所述巯基改性蓖麻油中,蓖麻油:3-巯基丙酸的质量比为10:(4-5);所述催化剂为对甲苯磺酸,加入量为蓖麻油质量的2.5-3wt%;所述稳定剂为对苯二酚,加入量为蓖麻油质量的0.5-1wt%。
进一步的,所述支化单体中,含酚羟基二苄叉丙酮:1,3,5-三氨基苯:多聚甲醛的质量比为(6-9):(2-3):(0.2-0.3)。
进一步的,所述复合防腐阻燃剂中,支化单体:六氯环三膦腈的质量比为(5-6):1;支化单体:无水碳酸钾的质量比为1:(0.7-0.8)。
进一步的,所述防火防腐涂料中各组分原料占比,按质量份数计,巯基改性蓖麻油80-120份,复合防腐阻燃剂60-90份,交联剂20-40份,2,4,6-三甲基-2,4,6-三乙烯基环三硅氮烷20-40份,2,2-二羟甲基丙酸1-2份。
进一步的,所述涂覆量为160-180g/m2。
与现有技术相比,本发明所达到的有益效果是:
本发明以自制的含酚羟基的二苄叉丙酮为基础化学支架,通过与1,3,5-三氨基苯上的胺基反应制备得到一种含有端酚羟基的苯并噁嗪结构的支化单体,接着以阻燃剂六氯环三膦腈为反应中心,将上述制备的支化单体接枝在六氯环三膦腈周围形成具有独特超支化结构的复合防腐阻燃剂。还以自制的含酚羟基的二苄叉丙酮为基础化学支架,通过与烯丙基缩水甘油醚上的环氧基团反应得到一种含有端烯烃基团的交联剂。
将复合防腐阻燃剂和交联剂加入巯基改性蓖麻油中,再加入2,4,6-三甲基-2,4,6-三乙烯基环三硅氮烷作为稀释剂制备得到的防腐防火涂料,在UV光固化作用下,复合防腐阻燃剂和交联剂中二苄叉丙酮结构中的两个双键结构发生1,2环加成反应,将复合防腐阻燃剂和交联剂分子链端紧密连接在一起,同时复合防腐阻燃剂分子链与复合防腐阻燃剂分子链之间,交联剂分子链与交联剂分子链之间也在光照作用下发生1,2环加成反应,使得交联固化结构更加紧密。不仅如此,当复合防腐阻燃剂和交联剂反应后,将端烯烃基团引入分子链段中,使其在于巯基改性蓖麻油反应过程中,复合防腐阻燃剂其分子链中羰基两侧烯烃结构与端烯烃结构同时与巯基改性蓖麻油分子链上的巯基发生巯基-烯点击化学反应,将分子链紧密连接在一起;交联剂分子链段中同样存在着羰基两侧烯烃结构与两侧端烯烃结构在与复合防腐阻燃剂反应交联的同时也在与巯基改性蓖麻油反应交联。为了降低防腐防火涂料整体粘度,使其具有良好的浸透力,能够使各组分分散更均匀的同时浸透入木材自身具有的天然多孔结构中,使得固化后形成的涂层不止浮于木材表面,具有“铆钉”结构作用,大大增强了涂层的附着力和硬度,使得经过防腐防火涂料处理后的木材具有优异的防腐、防火、耐磨、高附着的优异性能。
本发明以自制的含酚羟基的二苄叉丙酮为基础化学支架,将防腐苯并噁嗪防腐结构与六氯环三膦腈氮磷结构同时引入其中,解决了传统阻燃剂与防腐剂在基体中的分散问题。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
以下实施例中,对羟基苯甲醛购自上海阿拉丁生化科技股份有限公司,多聚甲醛购自上海阿拉丁生化科技股份有限公司,2,4,6-三甲基-2,4,6-三乙烯基环三硅氮烷购自上海瀚鸿科技股份有限公司,1,3,5-三氨基苯购自北京华威锐科化工有限公司,CAS:108-72-5,蓖麻油购自上海麦克林生化科技股份有限公司,其余原料均为市售。
实施例1:一种木材表面防火防腐处理工艺:S1:将10g蓖麻油、0.25g对甲苯磺酸和0.5g对苯二酚加入50mL甲苯中搅拌均匀,氮气氛围下加热至110℃,将4g3-巯基丙酸分4次每次间隔1小时加入,搅拌反应5h,冷却至25℃,真空旋蒸,得到巯基改性蓖麻油;
S2:将2g对羟基苯甲醛、4g无水氯化钙和0.5g三氟化硼乙醚加入15mL甲醇中,加热至50℃,将6.66g30wt%丙酮甲醇溶液在12h内加入反应体系中,保温反应1h,将反应物加入500mL去离子水中,过滤,80℃真空干燥12h,得到含酚羟基二苄叉丙酮;
S3:将6g含酚羟基二苄叉丙酮、2g1,3,5-三氨基苯、0.2g多聚甲醛加入10mL二氧六环中,在80℃下反应5h,40℃旋蒸5h,得到支化单体;将5g支化单体和1g六氯环三膦腈加入50mL四氢呋喃中,加入0.7g无水碳酸钾,氮气氛围下加热至75℃反应8h,过滤,旋蒸,提纯,得到复合防腐阻燃剂;
S4:将5g含酚羟基二苄叉丙酮、4g烯丙基缩水甘油醚、0.09g咪唑和0.025g丁基羟基甲苯依次加入氮气氛围反应容器中搅拌均匀,加热至100℃反应25min,继续加热至110-℃反应3h,最后加热至122℃反应1h,冷却至60℃在90℃沸点石油醚中沉淀,纯化,得到交联剂。
S5:将60g复合防腐阻燃剂、20g交联剂、20g2,4,6-三甲基-2,4,6-三乙烯基环三硅氮烷和1g2,2-二羟甲基丙酸依次加入100g巯基改性蓖麻油中搅拌均匀,得到防火防腐涂料;将防腐防火涂料均匀涂覆在木材表面,光固化,得到表面防火防腐层。
实施例2:一种木材表面防火防腐处理工艺:S1:将10g蓖麻油、0.25g对甲苯磺酸和0.5g对苯二酚加入50mL甲苯中搅拌均匀,氮气氛围下加热至110℃,将4g3-巯基丙酸分4次每次间隔1小时加入,搅拌反应5h,冷却至25℃,真空旋蒸,得到巯基改性蓖麻油;
S2:将2g对羟基苯甲醛、4g无水氯化钙和0.5g三氟化硼乙醚加入15mL甲醇中,加热至50℃,将6.66g30wt%丙酮甲醇溶液在12h内加入反应体系中,保温反应1h,将反应物加入500mL去离子水中,过滤,80℃真空干燥12h,得到含酚羟基二苄叉丙酮;
S3:将6g含酚羟基二苄叉丙酮、2g1,3,5-三氨基苯、0.2g多聚甲醛加入10mL二氧六环中,在80℃下反应5h,40℃旋蒸5h,得到支化单体;将5g支化单体和1g六氯环三膦腈加入50mL四氢呋喃中,加入0.7g无水碳酸钾,氮气氛围下加热至75℃反应8h,过滤,旋蒸,提纯,得到复合防腐阻燃剂;
S4:将5g含酚羟基二苄叉丙酮、4g烯丙基缩水甘油醚、0.09g咪唑和0.025g丁基羟基甲苯依次加入氮气氛围反应容器中搅拌均匀,加热至100℃反应25min,继续加热至110-℃反应3h,最后加热至122℃反应1h,冷却至60℃在90℃沸点石油醚中沉淀,纯化,得到交联剂。
S5:将75g复合防腐阻燃剂、25g交联剂、30g2,4,6-三甲基-2,4,6-三乙烯基环三硅氮烷和1g2,2-二羟甲基丙酸依次加入100g巯基改性蓖麻油中搅拌均匀,得到防火防腐涂料;将防腐防火涂料均匀涂覆在木材表面,光固化,得到表面防火防腐层。
实施例3:一种木材表面防火防腐处理工艺:S1:将10g蓖麻油、0.25g对甲苯磺酸和0.5g对苯二酚加入50mL甲苯中搅拌均匀,氮气氛围下加热至110℃,将4g3-巯基丙酸分4次每次间隔1小时加入,搅拌反应5h,冷却至25℃,真空旋蒸,得到巯基改性蓖麻油;
S2:将2g对羟基苯甲醛、4g无水氯化钙和0.5g三氟化硼乙醚加入15mL甲醇中,加热至50℃,将6.66g30wt%丙酮甲醇溶液在12h内加入反应体系中,保温反应1h,将反应物加入500mL去离子水中,过滤,80℃真空干燥12h,得到含酚羟基二苄叉丙酮;
S3:将6g含酚羟基二苄叉丙酮、2g1,3,5-三氨基苯、0.2g多聚甲醛加入10mL二氧六环中,在80℃下反应5h,40℃旋蒸5h,得到支化单体;将5g支化单体和1g六氯环三膦腈加入50mL四氢呋喃中,加入0.7g无水碳酸钾,氮气氛围下加热至75℃反应8h,过滤,旋蒸,提纯,得到复合防腐阻燃剂;
S4:将5g含酚羟基二苄叉丙酮、4g烯丙基缩水甘油醚、0.09g咪唑和0.025g丁基羟基甲苯依次加入氮气氛围反应容器中搅拌均匀,加热至100℃反应25min,继续加热至110-℃反应3h,最后加热至122℃反应1h,冷却至60℃在90℃沸点石油醚中沉淀,纯化,得到交联剂。
S5:将80g复合防腐阻燃剂、40g交联剂、40g2,4,6-三甲基-2,4,6-三乙烯基环三硅氮烷和2g2,2-二羟甲基丙酸依次加入100g巯基改性蓖麻油中搅拌均匀,得到防火防腐涂料;将防腐防火涂料均匀涂覆在木材表面,光固化,得到表面防火防腐层。
对比例1:一种木材表面防火防腐处理工艺:S1:将10g蓖麻油、0.25g对甲苯磺酸和0.5g对苯二酚加入50mL甲苯中搅拌均匀,氮气氛围下加热至110℃,将4g3-巯基丙酸分4次每次间隔1小时加入,搅拌反应5h,冷却至25℃,真空旋蒸,得到巯基改性蓖麻油;
S2:将2g对羟基苯甲醛、4g无水氯化钙和0.5g三氟化硼乙醚加入15mL甲醇中,加热至50℃,将6.66g30wt%丙酮甲醇溶液在12h内加入反应体系中,保温反应1h,将反应物加入500mL去离子水中,过滤,80℃真空干燥12h,得到含酚羟基二苄叉丙酮;
S3:将4g双酚A、2g1,3,5-三氨基苯、0.2g多聚甲醛加入10mL二氧六环中,在80℃下反应5h,40℃旋蒸5h,得到支化单体;将5g支化单体和1g六氯环三膦腈加入50mL四氢呋喃中,加入0.7g无水碳酸钾,氮气氛围下加热至75℃反应8h,过滤,旋蒸,提纯,得到复合防腐阻燃剂;
S4:将5g含酚羟基二苄叉丙酮、4g烯丙基缩水甘油醚、0.09g咪唑和0.025g丁基羟基甲苯依次加入氮气氛围反应容器中搅拌均匀,加热至100℃反应25min,继续加热至110-℃反应3h,最后加热至122℃反应1h,冷却至60℃在90℃沸点石油醚中沉淀,纯化,得到交联剂。
S5:将60g复合防腐阻燃剂、20g交联剂、20g2,4,6-三甲基-2,4,6-三乙烯基环三硅氮烷和1g2,2-二羟甲基丙酸依次加入100g巯基改性蓖麻油中搅拌均匀,得到防火防腐涂料;将防腐防火涂料均匀涂覆在木材表面,光固化,得到表面防火防腐层。
对比例2:一种木材表面防火防腐处理工艺:S1:将10g蓖麻油、0.25g对甲苯磺酸和0.5g对苯二酚加入50mL甲苯中搅拌均匀,氮气氛围下加热至110℃,将4g3-巯基丙酸分4次每次间隔1小时加入,搅拌反应5h,冷却至25℃,真空旋蒸,得到巯基改性蓖麻油;
S2:将2g对羟基苯甲醛、4g无水氯化钙和0.5g三氟化硼乙醚加入15mL甲醇中,加热至50℃,将6.66g30wt%丙酮甲醇溶液在12h内加入反应体系中,保温反应1h,将反应物加入500mL去离子水中,过滤,80℃真空干燥12h,得到含酚羟基二苄叉丙酮;
S3:将4g含酚羟基二苄叉丙酮、2g聚醚胺、0.2g多聚甲醛加入10mL二氧六环中,在80℃下反应5h,40℃旋蒸5h,得到支化单体;将5g支化单体和1g六氯环三膦腈加入50mL四氢呋喃中,加入0.7g无水碳酸钾,氮气氛围下加热至75℃反应8h,过滤,旋蒸,提纯,得到复合防腐阻燃剂;
S4:将5g含酚羟基二苄叉丙酮、4g烯丙基缩水甘油醚、0.09g咪唑和0.025g丁基羟基甲苯依次加入氮气氛围反应容器中搅拌均匀,加热至100℃反应25min,继续加热至110-℃反应3h,最后加热至122℃反应1h,冷却至60℃在90℃沸点石油醚中沉淀,纯化,得到交联剂。
S5:将60g复合防腐阻燃剂、20g交联剂、20g2,4,6-三甲基-2,4,6-三乙烯基环三硅氮烷和1g2,2-二羟甲基丙酸依次加入100g巯基改性蓖麻油中搅拌均匀,得到防火防腐涂料;将防腐防火涂料均匀涂覆在木材表面,光固化,得到表面防火防腐层。
对比例3:一种木材表面防火防腐处理工艺:S1:将10g蓖麻油、0.25g对甲苯磺酸和0.5g对苯二酚加入50mL甲苯中搅拌均匀,氮气氛围下加热至110℃,将4g3-巯基丙酸分4次每次间隔1小时加入,搅拌反应5h,冷却至25℃,真空旋蒸,得到巯基改性蓖麻油
S2:将2g对羟基苯甲醛、4g无水氯化钙和0.5g三氟化硼乙醚加入15mL甲醇中,加热至50℃,将6.66g30wt%丙酮甲醇溶液在12h内加入反应体系中,保温反应1h,将反应物加入500mL去离子水中,过滤,80℃真空干燥12h,得到含酚羟基二苄叉丙酮;
S3:将6g含酚羟基二苄叉丙酮、2g1,3,5-三氨基苯、0.2g多聚甲醛加入10mL二氧六环中,在80℃下反应5h,40℃旋蒸5h,得到支化单体;将5g支化单体和1g六氯环三膦腈加入50mL四氢呋喃中,加入0.7g无水碳酸钾,氮气氛围下加热至75℃反应8h,过滤,旋蒸,提纯,得到复合防腐阻燃剂;
S4:将5g双酚A、4g烯丙基缩水甘油醚、0.09g咪唑和0.025g丁基羟基甲苯依次加入氮气氛围反应容器中搅拌均匀,加热至100℃反应25min,继续加热至110-℃反应3h,最后加热至122℃反应1h,冷却至60℃在90℃沸点石油醚中沉淀,纯化,得到交联剂。
S5:将60g复合防腐阻燃剂、20g交联剂、20g2,4,6-三甲基-2,4,6-三乙烯基环三硅氮烷和1g2,2-二羟甲基丙酸依次加入100g巯基改性蓖麻油中搅拌均匀,得到防火防腐涂料;将防腐防火涂料均匀涂覆在木材表面,光固化,得到表面防火防腐层。
试验:垂直燃烧试验按照UL-94试验标准(ASTM D3801)进行,测试样品为160g/m2涂覆量,尺寸为100×10×4mm3的杉木,含水率为12.0%。
极限氧指数(LOI)试验按照标准ASTM D2863使用氧指数仪测量测试样品为160g/m2涂覆量,尺寸为150×10×6mm3的杉木,含水率为12.0%。
采用铅笔硬度仪对涂覆后的木材样品表面进行铅笔硬度测试,根据ASTM D3363-05评价UV固化涂层的硬度。
根据ASTM D3359-09,使用百格刀测量涂层木材样品表面涂层的附着力测试。使用具有5个齿、间隔1.0mm的百格刀在90°垂直涂覆木材样品表面的涂层绘制网格图案。3M胶带粘在涂层划伤网格区域的表面,并用橡皮擦来回擦拭,以确保与样品接触均匀,然后在90s后除去胶带。
防腐性能根据GB/T 13942.1-2009进行测试;选择尺寸为30×12×3mm3的杉木进行测试,将杉木干燥至绝干状态,在121℃、0.1MPa条件下灭菌15min,防止在菌丝覆盖的培养皿中,封口放置在25℃、相对湿度为75%的环境中保存8周,试验结束将木材表面清除干净后,在105℃下干燥至绝干状态,比较样品前后质量损失率。
表1 木材防腐防火处理性能测试
结论:实施例1-3制备得防腐防火涂料用于木材的防腐防火处理具有优异的防腐防火性能。对比例1使用传统双酚A替代含酚羟基二苄叉丙酮合成支化单体,导致涂层交联密度降低,各项性能下降;对比例2使用聚醚胺替代1,3,5-三氨基苯合成支化单体,无法形成支化结构,无法形成错综复杂的交联网络结构;对比例3使用传统双酚A替代含酚羟基二苄叉丙酮合成交联剂,导致涂层交联密度降低,各项性能下降。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (9)
1.一种木材表面防火防腐处理工艺,其特征在于:包含以下步骤:
S1:将含酚羟基二苄叉丙酮、1,3,5-三氨基苯、多聚甲醛加入二氧六环中,在80-85℃下反应5-6h,旋蒸,得到支化单体;将支化单体和六氯环三膦腈加入四氢呋喃中,加入无水碳酸钾,氮气氛围下加热至75-80℃反应8-9h,过滤,旋蒸,提纯,得到复合防腐阻燃剂;
S2:将复合防腐阻燃剂、交联剂、2,4,6-三甲基-2,4,6-三乙烯基环三硅氮烷和2,2-二羟甲基丙酸依次加入巯基改性蓖麻油中搅拌均匀,得到防火防腐涂料;将防腐防火涂料均匀涂覆在木材表面,光固化,得到表面防火防腐层;
所述交联剂制备方法包括以下步骤:
将含酚羟基二苄叉丙酮、烯丙基缩水甘油醚、咪唑和丁基羟基甲苯依次加入氮气氛围反应容器中搅拌均匀,加热至100-105℃反应25-30min,继续加热至110-115℃反应3-3.5h,最后加热至122-125℃反应1-1.5h,冷却沉淀,纯化,得到交联剂。
2.根据权利要求1所述的一种木材表面防火防腐处理工艺,其特征在于:所述含酚羟基二苄叉丙酮:烯丙基缩水甘油醚的质量比为(5-6):(4-5);所述咪唑加入量为含酚羟基二苄叉丙酮加入量的1.8-2.5wt%;所述丁基羟基甲苯加入量为含酚羟基二苄叉丙酮加入量的0.5-0.8wt%。
3.根据权利要求1所述的一种木材表面防火防腐处理工艺,其特征在于:所述巯基改性蓖麻油制备方法包括以下步骤:
将蓖麻油、催化剂和稳定剂加入甲苯中搅拌均匀,氮气氛围下加热至110-115℃,加入3-巯基丙酸搅拌反应5-6h,冷却,旋蒸,得到巯基改性蓖麻油。
4.根据权利要求3所述的一种木材表面防火防腐处理工艺,其特征在于:所述巯基改性蓖麻油中,蓖麻油:3-巯基丙酸的质量比为10:(4-5)。
5.根据权利要求3所述的一种木材表面防火防腐处理工艺,其特征在于:所述催化剂为对甲苯磺酸,加入量为蓖麻油质量的2.5-3wt%;所述稳定剂为对苯二酚,加入量为蓖麻油质量的0.5-1wt%。
6.根据权利要求1所述的一种木材表面防火防腐处理工艺,其特征在于:所述支化单体中,含酚羟基二苄叉丙酮:1,3,5-三氨基苯:多聚甲醛的质量比为(6-9):(2-3):(0.2-0.3)。
7.根据权利要求1所述的一种木材表面防火防腐处理工艺,其特征在于:所述复合防腐阻燃剂中,支化单体:六氯环三膦腈的质量比为(5-6):1;支化单体:无水碳酸钾的质量比为1:(0.7-0.8)。
8.根据权利要求1所述的一种木材表面防火防腐处理工艺,其特征在于:所述防火防腐涂料中各组分原料占比,按质量份数计,巯基改性蓖麻油80-120份,复合防腐阻燃剂60-90份,交联剂20-40份,2,4,6-三甲基-2,4,6-三乙烯基环三硅氮烷20-40份,2,2-二羟甲基丙酸1-2份。
9.根据权利要求1所述的一种木材表面防火防腐处理工艺,其特征在于:所述涂覆量为160-180g/m2。
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