CN106985237A - A kind of preparation method of wooden cultural relic dehydration shaping strengthening agent - Google Patents
A kind of preparation method of wooden cultural relic dehydration shaping strengthening agent Download PDFInfo
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- CN106985237A CN106985237A CN201710266477.8A CN201710266477A CN106985237A CN 106985237 A CN106985237 A CN 106985237A CN 201710266477 A CN201710266477 A CN 201710266477A CN 106985237 A CN106985237 A CN 106985237A
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- 230000018044 dehydration Effects 0.000 title claims abstract description 26
- 238000006297 dehydration reaction Methods 0.000 title claims abstract description 26
- 238000007493 shaping process Methods 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000005728 strengthening Methods 0.000 title description 7
- 239000003921 oil Substances 0.000 claims abstract description 28
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- 238000007596 consolidation process Methods 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000001993 wax Substances 0.000 claims abstract description 18
- 239000002023 wood Substances 0.000 claims abstract description 17
- 238000010025 steaming Methods 0.000 claims abstract description 10
- 239000004203 carnauba wax Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 17
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 14
- 239000000047 product Substances 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 10
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 8
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 6
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000013517 stratification Methods 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000000346 nonvolatile oil Substances 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 8
- 230000032683 aging Effects 0.000 abstract description 8
- 238000011049 filling Methods 0.000 abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 4
- 239000004408 titanium dioxide Substances 0.000 abstract description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 230000003260 anti-sepsis Effects 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 abstract description 2
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000413 hydrolysate Substances 0.000 abstract description 2
- 238000012423 maintenance Methods 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000001954 sterilising effect Effects 0.000 abstract description 2
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 2
- 230000002421 anti-septic effect Effects 0.000 abstract 1
- 235000019198 oils Nutrition 0.000 description 23
- 238000000034 method Methods 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 238000004513 sizing Methods 0.000 description 7
- 238000007654 immersion Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 244000055346 Paulownia Species 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 229930006000 Sucrose Natural products 0.000 description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 2
- 229940037003 alum Drugs 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 239000005720 sucrose Substances 0.000 description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 description 2
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 244000021150 Orbignya martiana Species 0.000 description 1
- 235000014643 Orbignya martiana Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 229940015043 glyoxal Drugs 0.000 description 1
- 238000005213 imbibition Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- B27K2240/00—Purpose of the treatment
- B27K2240/20—Removing fungi, molds or insects
-
- 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
- B27K2240/00—Purpose of the treatment
- B27K2240/70—Hydrophobation treatment
-
- 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
- B27K2240/00—Purpose of the treatment
- B27K2240/90—UV-protection
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Forests & Forestry (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
Abstract
The present invention relates to the preparation method of wooden cultural relic dehydration shaping consolidation process agent, belong to historical relic and reinforce preparing technical field.The present invention first fries Oleum Verniciae fordii and Brazil wax through steaming, purification, obtain wood wax oil, Oleum Verniciae fordii in wood wax oil can penetrate into inside historical relic, historical relic is carried out to moisten maintenance, and can antisepsis and sterilization, palm wax can be combined with the fibre compact of historical relic, increase the intensity of historical relic, and play a part of waterproof, it is hydrolyzed again by raw material of HMDO, its hydrolysate can be with the hydroxyl reaction in timber, silica dioxide gel is set to be combined closely in the form of chemical bond with timber, reduce the hydroscopicity of timber, titanium dioxide is equipped with again, titanium dioxide can increase the ageing-resistant performance of historical relic, wooden cultural relic dehydration shaping consolidation process agent prepared by the present invention can carry out dehydration filling to wooden cultural relic, antiseptic insect-repelling, reinforce, moistureproof and waterproof etc. is protected, life 6~8 years.
Description
Technical field
The present invention relates to the preparation method of wooden cultural relic dehydration shaping strengthening agent, belong to historical relic reinforcement technique field.
Background technology
Timber is widespread in nature, and it processes simple, is one of material that the mankind use earliest, therefore wooden text
Thing is one of most common historical relic in archaeology.Unearthed wooden cultural relic due to burying in underground, often containing a large amount of water for a long time
Point.Although surface is bright and new when being unearthed, due to being soaked for a long time in underground water, and decomposed by Soil Microorganism, in it
Rot in portion.Therefore, the dehydration shaping of waterlogged wooden culture relics is reinforced where the always heavy difficult point in wooden cultural relic protection field.
Although waterlogged wooden culture relics remain in that intact, its substantial internal polysaccharide component on the surface
（Cellulose and hemicellulose）Seriously degrade, cell wall structure is broken to can't bear, if before it is dried without appropriate dehydration
Consolidation process, will occur serious deformation, cracking and even damages.Traditional waterlogged wooden culture relics dehydration shaping reinforcement means includes
Alum method, sucrose method, resin method, polyethylene glycol method, alcohol ether connect leaching method and glyoxal method etc., but they have suction acid tide respectively
Solve, easily go mouldy, poor permeability, low intensity, strong toxicity the shortcomings of, therefore, still must be to explore better method and effort.
With flourishing for modern polymer science technology, synthesis polymer reactant is applied to historical relic more and more
Protection, specific in terms of waterlogged wooden culture relics protection.The use of synthesis macromolecule most efficient method is that monomer infiltration polymerize
Method, compared with the resin and polyethylene glycol of HMW, the monomer of small-molecular-weight is easier to penetrate into the inside of waterlogged wooden culture relics,
With more preferable penetration depth, processing time can be shortened；Compared with alum, sucrose, the polymer substance after polymerization has more preferable
Water proofing property and antibiotic property；Meanwhile, macromolecule modifiability is strong, can be easily modified as needed.But it is big
Many synthesis polymer reactants have ageing-resistant performance and the relatively poor weakness of water resistance, and reaction condition is relatively violent.Cause
This, is badly in need of finding a kind of method that water resistance is good, ageing-resistant performance is good to carry out being dehydrated anti-corrosion sizing consolidation process to historical relic.
The content of the invention
The technical problems to be solved by the invention：Synthesis height for being conventionally used to wooden cultural relic dehydration shaping consolidation process
There is provided a kind of preparation side of wooden cultural relic dehydration shaping strengthening agent for molecular agents water resistance and the shortcoming of loss of properties on aging
Method.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）The ripe bancoul nuts of 1~3kg are weighed, are placed under the sun after being exposed to the sun to bancoul nuts and splitting, through shelling, picking, wash,
Dry, crush and sieve, obtain sieving, sieving is placed in oil press, being 60~95 DEG C in temperature pushes expressed oil, obtains
To rough Oleum Verniciae fordii；
（2）Rough Oleum Verniciae fordii is filtered, filtrate is obtained, 400~500g filtrates and 300~400g Brazil waxs are steamed
Fry, will steam the material after frying is 1 in mass ratio with absolute ethyl alcohol:1~1:After 2 mixing, stratification obtains subnatant, by under
Layer liquid is distilled, and is removed absolute ethyl alcohol, is obtained wood wax oil；
（3）25~30g HMDOs are weighed to be added in three-necked flask, in temperature be 120~130 DEG C at backflow 40~
After 50min, then 25~30mL mass fractions are added dropwise for 35% phosphoric acid solution, 3~4h of stirring reaction, reaction terminates, and obtains product；
（4）Weigh 6~8g butyl titanates and 8~12g Boratexes are added in 100~200mL absolute ethyl alcohols, stirring and dissolving
Afterwards, mixed liquor is obtained, it is 35% that 15~20g products, 40~50g wood wax oils and 50~60mL mass fractions are added into mixed liquor
Adlerika, 1~2h of stirring reaction, you can obtain wooden cultural relic dehydration shaping consolidation process agent.
Step（2）When described filtrate and Brazil wax steam stir-fry, 20~30g rosin resins can also be added.
Step（2）The temperature that described steaming is fried is 120~130 DEG C, and the steaming stir-fry time is 15~20min.
Step（2）The temperature of described absolute ethyl alcohol is 0~5 DEG C.
Step（2）The temperature of described distillation is 80~85 DEG C, and vapo(u)rizing temperature is 30~40min.
Step（3）The drop rate of described phosphoric acid solution is 1~3mL/min.
The present invention is compared with other method, and advantageous effects are：
（1）The present invention obtains wood wax oil, wood wax oil by the way that Oleum Verniciae fordii, Brazil wax and rosin resin are carried out into steaming stir-fry, purification
In Oleum Verniciae fordii can penetrate into inside wooden cultural relic, historical relic is carried out to moisten maintenance, and can antisepsis and sterilization, the palm wax in wood wax oil
It can be combined with rosin resin with the fibre compact of wooden cultural relic, increase the intensity of historical relic, while waterproof can be played a part of；
（2）The present invention is hydrolyzed by raw material of HMDO, and its hydrolysate is silica dioxide gel, silica
Gel and then can make the form of silica dioxide gel and chemical bond and timber combine closely with the hydroxyl reaction in timber, so that
Strengthen the intensity of wooden cultural relic, and the free hydroxyl group in wooden cultural relic is reduced, water imbibition is reduced, then be equipped with titanium dioxide,
Titanium dioxide can increase the ageing-resistant performance of wooden cultural relic as ultraviolet light screener.
Embodiment
The ripe bancoul nuts of 1~3kg are weighed, is placed in being exposed to the sun to bancoul nuts under the sun and splits, the bancoul nuts split are gone
Shell, picks out bancoul nuts benevolence therein, and bancoul nuts benevolence is cleaned 3~5 times with water, and clean bancoul nuts benevolence is placed in baking oven,
It is that to dry to bancoul nuts benevolence moisture content under the conditions of 80~90 DEG C be 5~8% in temperature, dry bancoul nuts benevolence is placed in pulverizer
After middle crushing, 80~100 mesh sieves are crossed, sieving is obtained, sieving is placed in oil press, being 90~95 DEG C in temperature squeezes out
Oil, obtains rough Oleum Verniciae fordii, and rough Oleum Verniciae fordii is filtered, filtrate is obtained, and takes 400~500g filtrates, 300~400g babassus
Wax and 20~30g rosin resins are added in steaming stir-fry machine, and it is 120~130 DEG C to control to steam stir-fry machine temperature, and rotating speed is 150~200r/
Min, which steams, fries 15~20min, the absolute ethyl alcohol in mass ratio 1 that will steam the material after frying with temperature is 0~5 DEG C:1~1:2 mixing
Afterwards, stratification, obtains subnatant, and lower floor's oil phase is moved into distilling apparatus, and 30 are heated under the conditions of temperature is 80~85 DEG C
~40min, removes absolute ethyl alcohol, obtains wood wax oil, weighs 25~30g HMDOs and is added to thermometer and returns
In the three-necked flask for flowing device, flask is placed in water-bath, it is 120~130 DEG C to control bath temperature, flow back 40~50min
Afterwards, it is 35% phosphoric acid solution 25~30mL mass fractions to be added dropwise into flask, and it is 1~3mL/min to control drop rate, waits to be added dropwise
After finishing, 3~4h of stirring reaction, reaction terminates, and obtains product, weighs 6~8g butyl titanates and 8~12g Boratexes are added
Into the beaker for filling 100~200mL absolute ethyl alcohols, by beaker move into digital display constant temperature blender with magnetic force in, in temperature be 50~
60 DEG C, rotating speed is 20~30min of stirring and dissolving under 260~300r/min, obtains mixed liquor, and 15~20g is added into mixed liquor
Product, 40~50g wood wax oil and 50~60mL mass fractions are 35% Adlerika, and insulated and stirred reacts 1~2h, certainly
So it is cooled to room temperature, you can obtain wooden cultural relic dehydration shaping consolidation process agent.
Example 1
The ripe bancoul nuts of 1kg are weighed, is placed in being exposed to the sun to bancoul nuts under the sun and splits, the bancoul nuts split are shelled, picked
Go out bancoul nuts benevolence therein, bancoul nuts benevolence cleaned 3 times with water, clean bancoul nuts benevolence is placed in baking oven, in temperature be 80
It is 5% to be dried under the conditions of DEG C to bancoul nuts benevolence moisture content, dry bancoul nuts benevolence is placed in after being crushed in pulverizer, crosses 80 mesh sieves,
Sieving is obtained, sieving is placed in oil press, is that 90 DEG C of squeezings are fuel-displaced in temperature, rough Oleum Verniciae fordii is obtained, by rough paulownia
Seed oil filtering, obtains filtrate, takes 400g filtrates, 300g Brazil waxs and 20g rosin resins to be added in steaming stir-fry machine, control is steamed
Stir-fry machine temperature is 120 DEG C, and rotating speed is that 150r/min steams stir-fry 15min, will steam the material after frying and be pressed with temperature for 0 DEG C of absolute ethyl alcohol
Mass ratio 1:After 1 mixing, stratification obtains subnatant, and lower floor oil phase is moved into distilling apparatus, in temperature be 80 DEG C of conditions
Lower heating 30min, removes absolute ethyl alcohol, obtains wood wax oil, weighs 25g HMDOs and is added to thermometer and returns
In the three-necked flask for flowing device, flask is placed in water-bath, it is 120 DEG C to control bath temperature, after backflow 40min, to flask
Middle dropwise addition 25mL mass fractions are 35% phosphoric acid solution, controls drop rate for 1mL/min, after after completion of dropping, stirring reaction
3h, reaction terminates, and obtains product, weighs 6g butyl titanates and 8g Boratexes are added to the beaker for filling 100mL absolute ethyl alcohols
In, beaker is moved into digital display constant temperature blender with magnetic force, is 50 DEG C in temperature, rotating speed is stirring and dissolving 20min under 260r/min,
Mixed liquor is obtained, it is 35% Adlerika that 15g products, 40g wood wax oil and 50mL mass fractions are added into mixed liquor, is protected
Warm stirring reaction 1h, is naturally cooling to room temperature, you can obtain wooden cultural relic dehydration shaping consolidation process agent.
The wooden cultural relic for needing sizing consolidation process is put into tank, the wooden cultural relic then prepared with the present invention is dehydrated
Sizing consolidation process agent submerges wooden cultural relic, immersion treatment 2 days, then the wooden cultural relic after immersion is taken out and dried.
After testing, the wooden cultural relic hydroscopicity after wooden cultural relic dehydration shaping consolidation process agent processing prepared by the present invention is low, waterproof
Effect is good, and historical relic has good ageing-resistant performance after reinforcing, and life-span ratio is extended 6 years using conventional strengthening agent, thermal decomposition temperature
Degree brings up to 520.5 DEG C by 320.5 DEG C, and shrinkage factor is 5.30%.
Example 2
The ripe bancoul nuts of 2kg are weighed, is placed in being exposed to the sun to bancoul nuts under the sun and splits, the bancoul nuts split are shelled, picked
Go out bancoul nuts benevolence therein, bancoul nuts benevolence cleaned 4 times with water, clean bancoul nuts benevolence is placed in baking oven, in temperature be 85
It is 7% to be dried under the conditions of DEG C to bancoul nuts benevolence moisture content, dry bancoul nuts benevolence is placed in after being crushed in pulverizer, crosses 90 mesh sieves,
Sieving is obtained, sieving is placed in oil press, is that 93 DEG C of squeezings are fuel-displaced in temperature, rough Oleum Verniciae fordii is obtained, by rough paulownia
Seed oil filtering, obtains filtrate, takes 450g filtrates, 350g Brazil waxs and 25g rosin resins to be added in steaming stir-fry machine, control is steamed
Stir-fry machine temperature is 125 DEG C, and rotating speed is that 180r/min steams stir-fry 18min, will steam the material after frying and be pressed with temperature for 3 DEG C of absolute ethyl alcohol
Mass ratio 1:After 2 mixing, stratification obtains subnatant, and lower floor oil phase is moved into distilling apparatus, in temperature be 83 DEG C of conditions
Lower heating 35min, removes absolute ethyl alcohol, obtains wood wax oil, weighs 28g HMDOs and is added to thermometer and returns
In the three-necked flask for flowing device, flask is placed in water-bath, it is 125 DEG C to control bath temperature, after backflow 45min, to flask
Middle dropwise addition 28mL mass fractions are 35% phosphoric acid solution, controls drop rate for 2mL/min, after after completion of dropping, stirring reaction
4h, reaction terminates, and obtains product, weighs 7g butyl titanates and 10g Boratexes are added to the beaker for filling 150mL absolute ethyl alcohols
In, beaker is moved into digital display constant temperature blender with magnetic force, is 55 DEG C in temperature, rotating speed is stirring and dissolving 25min under 280r/min,
Mixed liquor is obtained, it is 35% Adlerika that 18g products, 45g wood wax oil and 55mL mass fractions are added into mixed liquor, is protected
Warm stirring reaction 2h, is naturally cooling to room temperature, you can obtain wooden cultural relic dehydration shaping consolidation process agent.
The wooden cultural relic for needing sizing consolidation process is put into tank, the wooden cultural relic then prepared with the present invention is dehydrated
Sizing consolidation process agent submerges wooden cultural relic, immersion treatment 2 days, then the wooden cultural relic after immersion is taken out and dried.
After testing, the wooden cultural relic hydroscopicity after wooden cultural relic dehydration shaping consolidation process agent processing prepared by the present invention is low, waterproof
Effect is good, and historical relic has good ageing-resistant performance after reinforcing, and life-span ratio is extended 7 years using conventional strengthening agent, thermal decomposition temperature
Degree brings up to 528.5 DEG C by 326.5 DEG C, and shrinkage factor is 5.23%.
Example 3
The ripe bancoul nuts of 3kg are weighed, is placed in being exposed to the sun to bancoul nuts under the sun and splits, the bancoul nuts split are shelled, picked
Go out bancoul nuts benevolence therein, bancoul nuts benevolence cleaned 5 times with water, clean bancoul nuts benevolence is placed in baking oven, in temperature be 90
It is 8% to be dried under the conditions of DEG C to bancoul nuts benevolence moisture content, dry bancoul nuts benevolence is placed in after being crushed in pulverizer, crosses 100 mesh
Sieve, obtains sieving, sieving is placed in oil press, is that 95 DEG C of squeezings are fuel-displaced in temperature, obtains rough Oleum Verniciae fordii, will be rough
Oleum Verniciae fordii is filtered, and obtains filtrate, takes 500g filtrates, 400g Brazil waxs and 30g rosin resins to be added in steaming stir-fry machine, control
It is 130 DEG C to steam stir-fry machine temperature, and rotating speed steams for 200r/min fries 20min, will steam the absolute ethyl alcohol that material and temperature after frying are 5 DEG C
In mass ratio 1:After 2 mixing, stratification obtains subnatant, and lower floor oil phase is moved into distilling apparatus, in temperature be 85 DEG C of bars
Heat 40min under part, remove absolute ethyl alcohol, obtain wood wax oil, weigh 30g HMDOs be added to thermometer and
In the three-necked flask of reflux, flask is placed in water-bath, it is 130 DEG C to control bath temperature, after backflow 50min, to burning
It is 35% phosphoric acid solution that 30mL mass fractions are added dropwise in bottle, control drop rate for 3mL/min, after after completion of dropping, stirring reaction
4h, reaction terminates, and obtains product, weighs 8g butyl titanates and 12g Boratexes are added to the beaker for filling 200mL absolute ethyl alcohols
In, beaker is moved into digital display constant temperature blender with magnetic force, is 60 DEG C in temperature, rotating speed is stirring and dissolving 30min under 300r/min,
Mixed liquor is obtained, it is 35% Adlerika that 20g products, 50g wood wax oil and 60mL mass fractions are added into mixed liquor, is protected
Warm stirring reaction 2h, is naturally cooling to room temperature, you can obtain wooden cultural relic dehydration shaping consolidation process agent.
The wooden cultural relic for needing sizing consolidation process is put into tank, the wooden cultural relic then prepared with the present invention is dehydrated
Sizing consolidation process agent submerges wooden cultural relic, immersion treatment 3 days, then the wooden cultural relic after immersion is taken out and dried.
After testing, the wooden cultural relic hydroscopicity after wooden cultural relic dehydration shaping consolidation process agent processing prepared by the present invention is low, waterproof
Effect is good, and historical relic has good ageing-resistant performance after reinforcing, and life-span ratio is extended 8 years using conventional strengthening agent, thermal decomposition temperature
Degree brings up to 531.5 DEG C by 332.5 DEG C, and shrinkage factor is 5.28%.
Claims (6)
1. a kind of preparation method of wooden cultural relic dehydration shaping consolidation process agent, it is characterised in that specifically preparation process is：
（1）The ripe bancoul nuts of 1~3kg are weighed, are placed under the sun after being exposed to the sun to bancoul nuts and splitting, through shelling, picking, wash,
Dry, crush and sieve, obtain sieving, sieving is placed in oil press, being 60~95 DEG C in temperature pushes expressed oil, obtains
To rough Oleum Verniciae fordii；
（2）Rough Oleum Verniciae fordii is filtered, filtrate is obtained, 400~500g filtrates and 300~400g Brazil waxs are steamed
Fry, will steam the material after frying is 1 in mass ratio with absolute ethyl alcohol:1~1:After 2 mixing, stratification obtains subnatant, by under
Layer liquid is distilled, and is removed absolute ethyl alcohol, is obtained wood wax oil；
（3）25~30g HMDOs are weighed to be added in three-necked flask, in temperature be 120~130 DEG C at backflow 40~
After 50min, then 25~30mL mass fractions are added dropwise for 35% phosphoric acid solution, 3~4h of stirring reaction, reaction terminates, and obtains product；
（4）Weigh 6~8g butyl titanates and 8~12g Boratexes are added in 100~200mL absolute ethyl alcohols, stirring and dissolving
Afterwards, mixed liquor is obtained, it is 35% that 15~20g products, 40~50g wood wax oils and 50~60mL mass fractions are added into mixed liquor
Adlerika, 1~2h of stirring reaction, you can obtain wooden cultural relic dehydration shaping consolidation process agent.
2. a kind of preparation method of wooden cultural relic dehydration shaping consolidation process agent according to claim 1, it is characterised in that：
Step（2）When described filtrate and Brazil wax steam stir-fry, 20~30g rosin resins can also be added.
3. a kind of preparation method of wooden cultural relic dehydration shaping consolidation process agent according to claim 1, it is characterised in that：
Step（2）The temperature that described steaming is fried is 120~130 DEG C, and the steaming stir-fry time is 15~20min.
4. a kind of preparation method of wooden cultural relic dehydration shaping consolidation process agent according to claim 1, it is characterised in that：
Step（2）The temperature of described absolute ethyl alcohol is 0~5 DEG C.
5. a kind of preparation method of wooden cultural relic dehydration shaping consolidation process agent according to claim 1, it is characterised in that：
Step（2）The temperature of described distillation is 80~85 DEG C, and vapo(u)rizing temperature is 30~40min.
6. a kind of preparation method of wooden cultural relic dehydration shaping consolidation process agent according to claim 1, it is characterised in that：
Step（3）The drop rate of described phosphoric acid solution is 1~3mL/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108393984A (en) * | 2018-02-22 | 2018-08-14 | 浙江大学 | A kind of waterlogged wooden culture relics composite consolidation material and preparation method thereof |
| CN113146765A (en) * | 2021-04-22 | 2021-07-23 | 贵州八六三科技有限公司 | Environment-friendly flame-retardant wood |
| CN116330419A (en) * | 2023-03-24 | 2023-06-27 | 北京大学 | Pretreatment method for freeze drying of saturated wooden cultural relics |
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| JPH0924506A (en) * | 1995-07-11 | 1997-01-28 | Hideo Yoshida | Unearthed cultural relic and its preservation treatment |
| CN103213180A (en) * | 2013-03-15 | 2013-07-24 | 西南林业大学 | Strengthening agent for wooden relics, and preparation method and application thereof |
| CN103612305A (en) * | 2013-11-07 | 2014-03-05 | 陕西师范大学 | Fireproofing and insect-proofing modifying liquid for collection tools of files and cultural relics and application of modifying liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH0924506A (en) * | 1995-07-11 | 1997-01-28 | Hideo Yoshida | Unearthed cultural relic and its preservation treatment |
| CN103213180A (en) * | 2013-03-15 | 2013-07-24 | 西南林业大学 | Strengthening agent for wooden relics, and preparation method and application thereof |
| CN103612305A (en) * | 2013-11-07 | 2014-03-05 | 陕西师范大学 | Fireproofing and insect-proofing modifying liquid for collection tools of files and cultural relics and application of modifying liquid |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108393984A (en) * | 2018-02-22 | 2018-08-14 | 浙江大学 | A kind of waterlogged wooden culture relics composite consolidation material and preparation method thereof |
| CN113146765A (en) * | 2021-04-22 | 2021-07-23 | 贵州八六三科技有限公司 | Environment-friendly flame-retardant wood |
| CN116330419A (en) * | 2023-03-24 | 2023-06-27 | 北京大学 | Pretreatment method for freeze drying of saturated wooden cultural relics |
| CN116330419B (en) * | 2023-03-24 | 2023-09-26 | 北京大学 | Pretreatment method for freeze drying of saturated wooden cultural relics |
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