CN108559334A - A method of improving fluorescent dye tinctorial property on timber - Google Patents
A method of improving fluorescent dye tinctorial property on timber Download PDFInfo
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- CN108559334A CN108559334A CN201810379149.3A CN201810379149A CN108559334A CN 108559334 A CN108559334 A CN 108559334A CN 201810379149 A CN201810379149 A CN 201810379149A CN 108559334 A CN108559334 A CN 108559334A
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- fluorescent dye
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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
- C09D15/00—Woodstains
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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
- B27K5/00—Treating of wood not provided for in groups B27K1/00, B27K3/00
- B27K5/02—Staining or dyeing wood; Bleaching wood
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Forests & Forestry (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
Abstract
The present invention relates to wood processing treatment technical fields,Disclose a kind of method improving fluorescent dye tinctorial property on timber,Activating agent and metal salt are added in fluorescent dye,The nitrogen nitrogen ethyl diacetate compound of chimeric graphene oxide can form the colloid beam of sequential combination,Make the effect of power between generation dipole between fluorescent dye and lumber fibre,Improve fiber affinity,Dyestuff can penetrate into wood internal,With photostability outstanding and thermal stability,Activating agent can excite the group with Absorption Characteristics frequencies of light that electron transition occurs,Improve quantum yield,Reduce the energy loss generated due to intramolecular warm-up movement,Chromophore is induced to be converted to fluorogen,With fabulous fastness to light,Fastness to sublimation and light fastness,In addition to this,It can also be with the amino in fiber,Hydroxyl,The groups cross-linking reaction such as amide groups,To improve moisture-proof firmness.
Description
Technical field
The invention belongs to wood processing treatment technical fields, and in particular to a kind of raising fluorescent dye coloring on timber
The method of energy.
Background technology
Woodwork refers to after mechanically or chemically processing, still keeping wood-based using timber or wood materials as raw material
The industrial products of this characteristic, since woodwork has, light-weight, elasticity is good, beautiful texture, is comfortable on, environmentally friendly, easy
In the processing the features such as, and timber resources reproducible utilization, therefore, it has become, and the mankind are most important, most widely used raw material
One of.In most common four big material of mankind nowadays(Steel, timber, cement, plastics)In, timber with its distinctive matter, line,
The characteristics such as color, taste, and receive liking for people.
Wood staining technology application starts from, hereafter, basic theories and technology of many scholars to wood staining in 1913
A large amount of research has been done, the functionization of wood staining technology and industrialization is made to have obtained rapid development.Wood staining is to improve
The one side of wood visual is one of the approach of decoration, the grain of wood can be made relatively sharp pleasing after dyeing processing,
Enhance the decorative effect of woodwork appearance colour.Current fluorescent dye is applied in every field, can not only be obtained beautiful in colour
Decorative effect, also act powerful function affect, and still seldom in the application in wood staining field, fluorescent dye is only
Can brush in wood surface, wood internal can not be penetrated into, be easy rubbed off, color is very unstable, be illuminated by the light and
Climatic effect can occur to change colour and fade.
Invention content
The purpose of the present invention is for existing problem, provide a kind of raising fluorescent dye tinctorial property on timber
Method makes the effect of power between generation dipole between fluorescent dye and lumber fibre, improves fiber affinity, dyestuff can permeate
To wood internal, there is photostability outstanding and thermal stability.
The present invention is achieved by the following technical solutions:
A method of fluorescent dye tinctorial property on timber is improved, fluorescent dye is dissolved in having for 2.0-2.2 times of volume
In solvent, the modifying agent for accounting for fluorescent dye quality 1.8-2.0% is then added, 30- is mixed under 400-500 revs/min
It 40 minutes, is then placed in 55-60 DEG C of water-bath heating stirring 1.5-2.0 hours, is stored after cooling, the modifying agent is according to weight
Amount part meter consists of the following compositions:12-15 parts of activating agent, 1.5-1.8 parts of metal salt, 3.0-3.5 parts of ammonium nitrate solution, stearic acid
1.0-1.5 parts, 18-20 parts of ethyl alcohol, 0.5-0.8 parts of silane coupling agent, 1.0-1.2 parts of auxiliary agent;The preparation method of the activating agent
Include the following steps:
(1)Four-hole boiling flask equipped with blender, reflux condensing tube, thermometer, dropping funel is put into water-bath, is weighed
0.18-0.20 moles of N-N- diethyl alcohol radical aniline and 0.25-0.30 moles of phthalic acid are placed in four round flask, are added
3.5-3.8 grams of graphite powder is slowly added to the 15-20 milliliters of concentrated sulfuric acids, continues to stir after dripping while stirring under condition of ice bath
It mixes, temperature is in 0-5 DEG C of range in control flask;
(2)It waits for that the heat consumption that reaction generates is complete, after temperature no longer rises, 2.0-2.5 grams of potassium permanganate is added, stirs 30-40
Minute, under nitrogen protection, 8-10 milliliters of dimethylformamides are added dropwise, reaction system is heated to 70-80 DEG C after dripping,
Reflux is stirred to react 4-5 hours under nitrogen protection, naturally cools to 25-28 DEG C after reaction, and sodium carbonate regulation system is added
Reaction solution is placed in ice-water bath by pH value in 6.8-7.0 ranges, stands 20-24 hours, with deionized water centrifuge washing to molten
Sulfate radical-free ion in liquid finally uses Rotary Evaporators rotary evaporation to remove moisture.
It is further described as to said program, the organic solvent can dissolve corresponding fluorescent dye.
It is further described as to said program, the metal salt is consisted of the following compositions according to mass percent meter:
Copper chlorate accounts for that 15-20%, dichloride account for 18-22% suddenly, iron chloride accounts for 25-30%, remaining as sodium chloride.
It is further described as to said program, the ammonium nitrate solution mass concentration is 40-45%.
It is further described as to said program, the auxiliary agent contains following component according to mass percent meter:Defoaming
Agent accounts for 12-15%, preservative accounts for 20-25%, levelling agent accounts for 25-30%, remaining as thickener.
It is further described as to said program, step(1)The graphite powder particle size is between 40-50 microns.
It is further described as to said program, step(1)The concentrated sulfuric acid mass concentration is 96-98%.
The present invention has the following advantages compared with prior art:In order to solve existing fluorescent dye tinctorial property difference on woodwork
Problem, the present invention provides a kind of methods improving fluorescent dye tinctorial property on timber, and activity is added in fluorescent dye
The nitrogen nitrogen ethyl diacetate compound of agent and metal salt, chimeric graphene oxide can form the colloid beam of sequential combination, make glimmering
The effect that power between dipole is generated between photoinitiator dye and lumber fibre, improves fiber affinity, dyestuff can penetrate into timber
There is photostability outstanding and thermal stability, activating agent can excite the group with Absorption Characteristics frequencies of light that electricity occurs in portion
Sub- transition improves quantum yield, reduces the energy loss generated due to intramolecular warm-up movement, and induction chromophore turns to fluorogen
Change, have fabulous fastness to light, fastness to sublimation and light fastness, in addition to this, moreover it is possible to in fiber amino, hydroxyl,
The groups cross-linking reaction such as amide groups, to improve moisture-proof firmness, the present invention can improve the dye-uptake of fluorescent dye to 94%
More than, quantum yield is close to 1, and for single photon fluorescence excitation wavelength between 410-420 nanometers, fluorescence intensity is high in fluorescence spectra
Have horizontal 1.5 times, fluorescence property not by rub, clean, solarization is influenced, expanded fluorescent chemicals in timber field
Using.
Specific implementation mode
To make the purpose of the present invention, technical solution and effect clearer, clear and definite, with reference to specific embodiment to this hair
It is bright to be described further, it should be understood that the specific embodiments described herein are merely illustrative of the present invention, is not used to limit
Technical solution provided by the present invention.
Embodiment 1
A method of fluorescent dye tinctorial property on timber is improved, fluorescent dye is dissolved in the organic molten of 2.0 times of volumes
In agent, the modifying agent for accounting for fluorescent dye quality 1.8% is then added, is mixed 30 minutes under 400 revs/min, is then placed in
Heating stirring 1.5 hours in 55 DEG C of water-baths is stored after cooling, and the modifying agent consists of the following compositions in parts by weight:
12 parts of activating agent, 1.5 parts of metal salt, 3.0 parts of ammonium nitrate solution, 1.0 parts of stearic acid, 18 parts of ethyl alcohol, 0.5 part of silane coupling agent,
1.0 parts of auxiliary agent;The preparation method of the activating agent includes the following steps:
(1)Four-hole boiling flask equipped with blender, reflux condensing tube, thermometer, dropping funel is put into water-bath, weighs 0.18
Mole N-N- diethyl alcohol radical aniline and 0.25 mole of phthalic acid are placed in four round flask, 3.5 grams of graphite powders are added, in ice
Under the conditions of bath, it is slowly added to 15 milliliters of concentrated sulfuric acids while stirring, continues to stir after dripping, temperature is at 0-5 DEG C in control flask
Range;
(2)It waits for that the heat consumption that reaction generates is complete, after temperature no longer rises, 2.0 grams of potassium permanganate is added, stir 30 minutes,
Under nitrogen protection, 8 milliliters of dimethylformamides are added dropwise, reaction system is heated to 70 DEG C after dripping, is returned under nitrogen protection
Stream is stirred to react 4 hours, naturally cools to 25 DEG C after reaction, sodium carbonate regulation system pH value is added in 6.8-7.0 ranges,
Reaction solution is placed in ice-water bath, stands 20 hours, with sulfate radical-free ion in deionized water centrifuge washing to solution, finally
Moisture is removed with Rotary Evaporators rotary evaporation.
It is further described as to said program, the organic solvent can dissolve corresponding fluorescent dye.
It is further described as to said program, the metal salt is consisted of the following compositions according to mass percent meter:
Copper chlorate, which accounts for 15%, dichloride and accounts for 18%, iron chloride suddenly, accounts for 25%, remaining as sodium chloride.
It is further described as to said program, the ammonium nitrate solution mass concentration is 40%.
It is further described as to said program, the auxiliary agent contains following component according to mass percent meter:Defoaming
Agent, which accounts for 12%, preservative and accounts for 20%, levelling agent, accounts for 25%, remaining as thickener.
It is further described as to said program, step(1)The graphite powder particle size is between 40-50 microns.
It is further described as to said program, step(1)The concentrated sulfuric acid mass concentration is 96%.
Embodiment 2
A method of fluorescent dye tinctorial property on timber is improved, fluorescent dye is dissolved in the organic molten of 2.1 times of volumes
In agent, the modifying agent for accounting for fluorescent dye quality 1.9% is then added, is mixed 35 minutes under 450 revs/min, is then placed in
Heating stirring 1.8 hours in 58 DEG C of water-baths is stored after cooling, and the modifying agent consists of the following compositions in parts by weight:
13 parts of activating agent, 1.6 parts of metal salt, 3.3 parts of ammonium nitrate solution, 1.3 parts of stearic acid, 19 parts of ethyl alcohol, 0.6 part of silane coupling agent,
1.1 parts of auxiliary agent;The preparation method of the activating agent includes the following steps:
(1)Four-hole boiling flask equipped with blender, reflux condensing tube, thermometer, dropping funel is put into water-bath, weighs 0.19
Mole N-N- diethyl alcohol radical aniline and 0.28 mole of phthalic acid are placed in four round flask, 3.6 grams of graphite powders are added, in ice
Under the conditions of bath, it is slowly added to 18 milliliters of concentrated sulfuric acids while stirring, continues to stir after dripping, temperature is at 0-5 DEG C in control flask
Range;
(2)It waits for that the heat consumption that reaction generates is complete, after temperature no longer rises, 2.2 grams of potassium permanganate is added, stir 35 minutes,
Under nitrogen protection, 9 milliliters of dimethylformamides are added dropwise, reaction system is heated to 75 DEG C after dripping, is returned under nitrogen protection
Stream is stirred to react 4.5 hours, naturally cools to 26 DEG C after reaction, and sodium carbonate regulation system pH value is added in 6.8-7.0 models
It encloses, reaction solution is placed in ice-water bath, stand 22 hours, with sulfate radical-free ion in deionized water centrifuge washing to solution,
Finally Rotary Evaporators rotary evaporation is used to remove moisture.
It is further described as to said program, the organic solvent can dissolve corresponding fluorescent dye.
It is further described as to said program, the metal salt is consisted of the following compositions according to mass percent meter:
Copper chlorate, which accounts for 18%, dichloride and accounts for 20%, iron chloride suddenly, accounts for 28%, remaining as sodium chloride.
It is further described as to said program, the ammonium nitrate solution mass concentration is 43%.
It is further described as to said program, the auxiliary agent contains following component according to mass percent meter:Defoaming
Agent, which accounts for 13%, preservative and accounts for 23%, levelling agent, accounts for 28%, remaining as thickener.
It is further described as to said program, step(1)The graphite powder particle size is between 40-50 microns.
It is further described as to said program, step(1)The concentrated sulfuric acid mass concentration is 97%.
Embodiment 3
A method of fluorescent dye tinctorial property on timber is improved, fluorescent dye is dissolved in the organic molten of 2.2 times of volumes
In agent, the modifying agent for accounting for fluorescent dye quality 2.0% is then added, is mixed 40 minutes under 500 revs/min, is then placed in
Heating stirring 2.0 hours in 60 DEG C of water-baths is stored after cooling, and the modifying agent consists of the following compositions in parts by weight:
15 parts of activating agent, 1.8 parts of metal salt, 3.5 parts of ammonium nitrate solution, 1.5 parts of stearic acid, 20 parts of ethyl alcohol, 0.8 part of silane coupling agent,
1.2 parts of auxiliary agent;The preparation method of the activating agent includes the following steps:
(1)Four-hole boiling flask equipped with blender, reflux condensing tube, thermometer, dropping funel is put into water-bath, weighs 0.20
Mole N-N- diethyl alcohol radical aniline and 0.30 mole of phthalic acid are placed in four round flask, 3.8 grams of graphite powders are added, in ice
Under the conditions of bath, it is slowly added to 20 milliliters of concentrated sulfuric acids while stirring, continues to stir after dripping, temperature is at 0-5 DEG C in control flask
Range;
(2)It waits for that the heat consumption that reaction generates is complete, after temperature no longer rises, 2.5 grams of potassium permanganate is added, stir 40 minutes,
Under nitrogen protection, 10 milliliters of dimethylformamides are added dropwise, reaction system is heated to 80 DEG C after dripping, is returned under nitrogen protection
Stream is stirred to react 5 hours, naturally cools to 28 DEG C after reaction, sodium carbonate regulation system pH value is added in 6.8-7.0 ranges,
Reaction solution is placed in ice-water bath, stands 24 hours, with sulfate radical-free ion in deionized water centrifuge washing to solution, finally
Moisture is removed with Rotary Evaporators rotary evaporation.
It is further described as to said program, the organic solvent can dissolve corresponding fluorescent dye.
It is further described as to said program, the metal salt is consisted of the following compositions according to mass percent meter:
Copper chlorate, which accounts for 20%, dichloride and accounts for 22%, iron chloride suddenly, accounts for 30%, remaining as sodium chloride.
It is further described as to said program, the ammonium nitrate solution mass concentration is 45%.
It is further described as to said program, the auxiliary agent contains following component according to mass percent meter:Defoaming
Agent, which accounts for 15%, preservative and accounts for 25%, levelling agent, accounts for 30%, remaining as thickener.
It is further described as to said program, step(1)The graphite powder particle size is between 40-50 microns.
It is further described as to said program, step(1)The concentrated sulfuric acid mass concentration is 98%.
Comparative example 1
With differing only in for embodiment 1, the preparation addition of activating agent is omitted in modifying agent, remaining is consistent.
Comparative example 2
With differing only in for embodiment 2, the addition of metal salt, ammonium nitrate solution is omitted in modifying agent, remaining is consistent.
Comparative example 3
With differing only in for embodiment 3, activating agent omits the addition of graphite powder in preparing, remaining is consistent.
Contrast experiment
The method for using embodiment 1-3 and comparative example 1-3 respectively improves the tinctorial property of fluorescent dye, while setting is not added and changed
Property agent contrast test as a control group, keep each group irrelevant variable it is consistent, using alkaline rhodamine B as fluorescent dye, ethyl alcohol
As solvent, dye dosage 0.5%(Dyestuff accounts for wood weight ratio), adjusting pH value using sodium acetate-hac buffer is
6.0, prepare dye liquor, bath raio 1:150, it is stirred 30 minutes using high speed beater, reuses sand mill and carry out frosted, with poplar
Plank cuts into the light sheet that size is 5 centimetres * 5 centimetres * 3 centimetres, respectively at 25 DEG C, 35 DEG C, 45 DEG C as experimental subjects
Enter dye, dyeing time is 60 minutes, after wash and dries 2-3 hours, by fluorescent dye results of property record such as 1 institute of table
Show.
The dye-uptake of 1 each group sample of table fluorescent dye at different temperatures(%)
Shown by a series of experiments:The present invention can improve the dye-uptake of fluorescent dye to 94% or more, and quantum yield is close
1, for single photon fluorescence excitation wavelength between 410-420 nanometers, fluorescence intensity is higher by the 1.5 of existing level in fluorescence spectra
Times, fluorescence property not by rub, clean, solarization is influenced, expanded application of the fluorescent chemicals in timber field.
Claims (7)
1. a kind of method improving fluorescent dye tinctorial property on timber, which is characterized in that fluorescent dye is dissolved in 2.0-
In the organic solvent of 2.2 times of volumes, the modifying agent for accounting for fluorescent dye quality 1.8-2.0% is then added, at 400-500 revs/min
Lower mixing 30-40 minutes is then placed in 55-60 DEG C of water-bath heating stirring 1.5-2.0 hours, is stored after cooling, institute
Modifying agent is stated to consist of the following compositions in parts by weight:12-15 parts of activating agent, 1.5-1.8 parts of metal salt, ammonium nitrate solution
3.0-3.5 parts, 1.0-1.5 parts of stearic acid, 18-20 parts of ethyl alcohol, 0.5-0.8 parts of silane coupling agent, 1.0-1.2 parts of auxiliary agent;It is described
The preparation method of activating agent includes the following steps:
(1)Four-hole boiling flask equipped with blender, reflux condensing tube, thermometer, dropping funel is put into water-bath, is weighed
0.18-0.20 moles of N-N- diethyl alcohol radical aniline and 0.25-0.30 moles of phthalic acid are placed in four round flask, are added
3.5-3.8 grams of graphite powder is slowly added to the 15-20 milliliters of concentrated sulfuric acids, continues to stir after dripping while stirring under condition of ice bath
It mixes, temperature is in 0-5 DEG C of range in control flask;
(2)It waits for that the heat consumption that reaction generates is complete, after temperature no longer rises, 2.0-2.5 grams of potassium permanganate is added, stirs 30-40
Minute, under nitrogen protection, 8-10 milliliters of dimethylformamides are added dropwise, reaction system is heated to 70-80 DEG C after dripping,
Reflux is stirred to react 4-5 hours under nitrogen protection, naturally cools to 25-28 DEG C after reaction, and sodium carbonate regulation system is added
Reaction solution is placed in ice-water bath by pH value in 6.8-7.0 ranges, stands 20-24 hours, with deionized water centrifuge washing to molten
Sulfate radical-free ion in liquid finally uses Rotary Evaporators rotary evaporation to remove moisture.
2. a kind of method improving fluorescent dye tinctorial property on timber as described in claim 1, which is characterized in that described to have
Solvent can dissolve corresponding fluorescent dye.
3. a kind of method improving fluorescent dye tinctorial property on timber as described in claim 1, which is characterized in that the gold
Belong to salt to consist of the following compositions according to mass percent meter:Copper chlorate accounts for that 15-20%, dichloride account for 18-22% suddenly, iron chloride accounts for
25-30%, remaining as sodium chloride.
4. a kind of method improving fluorescent dye tinctorial property on timber as described in claim 1, which is characterized in that the nitre
Acid ammonium solution mass concentration is 40-45%.
5. a kind of method improving fluorescent dye tinctorial property on timber as described in claim 1, which is characterized in that described to help
Agent contains following component according to mass percent meter:Antifoaming agent accounts for 12-15%, preservative accounts for 20-25%, levelling agent accounts for 25-30%,
Remaining as thickener.
6. a kind of method improving fluorescent dye tinctorial property on timber as described in claim 1, which is characterized in that step
(1)The graphite powder particle size is between 40-50 microns.
7. a kind of method improving fluorescent dye tinctorial property on timber as described in claim 1, which is characterized in that step
(1)The concentrated sulfuric acid mass concentration is 96-98%.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110802697A (en) * | 2019-10-22 | 2020-02-18 | 含山县宏达门业家具有限公司 | Method for improving dyeing performance of hard wooden door |
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GB510761A (en) * | 1937-08-25 | 1939-08-08 | British Celanese | Improvements in or relating to the colouration of artificial textile materials |
CN105345904A (en) * | 2015-11-04 | 2016-02-24 | 安徽美景工艺品有限公司 | Oxidized graphene-silica sol enhanced pretreating agent for wicker for wickerwork and preparation method of oxidized graphene-silica sol enhanced pretreating agent |
CN107287883A (en) * | 2017-07-26 | 2017-10-24 | 山东圣泉新材料股份有限公司 | A kind of preparation method of modified cotton fiber, obtained product and purposes |
CN107417952A (en) * | 2017-07-28 | 2017-12-01 | 华北电力大学(保定) | A kind of cellulose fluorescent film and preparation method thereof |
-
2018
- 2018-04-25 CN CN201810379149.3A patent/CN108559334B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB510761A (en) * | 1937-08-25 | 1939-08-08 | British Celanese | Improvements in or relating to the colouration of artificial textile materials |
CN105345904A (en) * | 2015-11-04 | 2016-02-24 | 安徽美景工艺品有限公司 | Oxidized graphene-silica sol enhanced pretreating agent for wicker for wickerwork and preparation method of oxidized graphene-silica sol enhanced pretreating agent |
CN107287883A (en) * | 2017-07-26 | 2017-10-24 | 山东圣泉新材料股份有限公司 | A kind of preparation method of modified cotton fiber, obtained product and purposes |
CN107417952A (en) * | 2017-07-28 | 2017-12-01 | 华北电力大学(保定) | A kind of cellulose fluorescent film and preparation method thereof |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110802697A (en) * | 2019-10-22 | 2020-02-18 | 含山县宏达门业家具有限公司 | Method for improving dyeing performance of hard wooden door |
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