CN106956341A - A kind of attapulgite wood fire retardant and preparation method thereof - Google Patents
A kind of attapulgite wood fire retardant and preparation method thereof Download PDFInfo
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- CN106956341A CN106956341A CN201710231030.7A CN201710231030A CN106956341A CN 106956341 A CN106956341 A CN 106956341A CN 201710231030 A CN201710231030 A CN 201710231030A CN 106956341 A CN106956341 A CN 106956341A
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- attapulgite
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- fire retardant
- containing compound
- wood fire
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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
-
- 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
- B27K2240/30—Fireproofing
Abstract
The invention discloses a kind of attapulgite wood fire retardant and preparation method thereof, it is related to attapulgite processing technique field, includes the raw material of following part meter：1 ~ 3 part of 150 ~ 200 parts of attapulgite, 10 ~ 15 parts of phosphorus-containing compound, 10 ~ 15 parts of amino-compound, 10 ~ 15 parts of boron-containing compound, 10 ~ 15 parts of aluminium salt, 2 ~ 8 parts of surfactant, 1 ~ 3 part of antimony oxide and silicon dioxide gel.The present invention is using attapulgite as primary raw material, and preparation method is simple, good flame retardation effect, and the fire-retardant load medicine for timber is handled.
Description
Technical field
The present invention relates to attapulgite processing technique field, and in particular to a kind of attapulgite wood fire retardant and its preparation
Method.
Background technology
Timber is important Industrial Engineering material, and the ratio of construction and decoration timber total flow becomes in rising year by year
Gesture.But, undressed timber and its product are red label goods, there is disaster hidden-trouble.According to the fire statistics of countries in the world
Analysis, there is relevant with timber in 21% fire.In order to reduce fire, many countries are with the substantive requirements of form of law to making
Timber must carry out flame retardant treatment, and fire-retarding of wood is often handled with fire retardant, but in existing wood fire retardant, it is organic
Fire retardant is used because releasing a large amount of toxic gases when it burns and expensive without advocating；Resin type fire retardant, due to fire-retardant
Performance is not ideal enough and there are problems that impregnating difficult, processing material, is not widely used, at present using most extensive
Inorganic combustion inhibitor, have the advantages that wide material sources, price are low, asepsis environment-protecting, but at present many inorganic combustion inhibitors to timber
Flame retardant effect is not obvious, and leach resistance is poor, and deformation is big.
Attapulgite is a kind of silicate mineral for the magnalium containing Shuifu County for having layer chain, and its microstructure includes 3 levels：
（1）, basic structural unit be bar-like single crystal body, the brilliant a diameter of 0.01 μm of order of magnitude of rod, length is up to 0.1-1 μm；（2）, by list
The brilliant beam of the rod of brilliant aggregate parallel；（3）, mutually assembled as brilliant beam pile up formed by various aggregations, particle diameter is usually
The 0.01-0.1mm orders of magnitude.There is a small amount of research using attapulgite as the fire retardant raw material side of high molecular polymer at present, still
Effect is undesirable.
The content of the invention
It is main using attapulgite it is an object of the invention to provide a kind of attapulgite wood fire retardant and preparation method thereof
Raw material, preparation method is simple, good flame retardation effect, and the fire-retardant load medicine for timber is handled.
The invention provides following technical scheme：A kind of attapulgite wood fire retardant, includes the raw material of following part meter：
150 ~ 200 parts of attapulgite, 10 ~ 15 parts of phosphorus-containing compound, 10 ~ 15 parts of amino-compound, 10 ~ 15 parts of boron-containing compound,
1 ~ 3 part of 10 ~ 15 parts of aluminium salt, 2 ~ 8 parts of surfactant, 1 ~ 3 part of antimony oxide and silicon dioxide gel.
Preferably, by weight including 175 parts of attapulgite, 12 parts of phosphorus-containing compound, 12 parts of amino-compound, boracic
2 parts of 12 parts of compound, 12 parts of aluminium salt, 5 parts of surfactant, 2 parts of antimony oxide and silicon dioxide gel.
Preferably, the phosphorus-containing compound be phosphoric acid, phosphorous acid, hypophosphorous acid, pyrophosphoric acid, APP, diammonium hydrogen phosphate,
Any of ammonium dihydrogen phosphate.
Preferably, the amino-compound is dicyandiamide or urea.
Preferably, the boron-containing compound is any of boric acid, borax, sodium tetraborate, borate.
Preferably, the aluminium salt is any of aluminium chloride, aluminum sulfate, aluminum nitrate.
The present invention also provides a kind of preparation method of attapulgite wood fire retardant, comprises the following steps：
Step（1）, take attapulgite to be ground to crush to obtain attapulgite powder, 10 ~ 15 weights are poured into attapulgite powder
The clear water of amount times, the mixed liquor that 5 ~ 10min of high-speed stirred is obtained under the conditions of 1000 ~ 1200r/min of rotating speed stands 50 ~ 60min
Heated afterwards, heating-up temperature is 60 ~ 85 DEG C, and the heat time is 20 ~ 30min, drying process is carried out after heating and is obtained after purification
Attapulgite powder；
Step（2）, using 10 ~ 25keV, 30 ~ 35kG nitrogen ion beam is to step（1）Attapulgite powder after the purification of middle gained
End carries out radiation treatment, and attapulgite rod crystalline substance is broken up into dissociation；
Step（3）, by step（2）Attapulgite powder after radiation treatment adds the ethanol solution that mass concentration is 10 ~ 15%
In, 15 ~ 25min is stirred with 200 ~ 300r/min of rotating speed, then by ultrasonically treated, higher suspension attapulgite ethanol is obtained after standing
Suspension, filtering, it is 6 ~ 8 to be washed to pH value, refilters, is dried to obtain activation attapulgite powder；
Step（4）, phosphorus-containing compound, amino-compound, boron-containing compound, aluminium salt, surfactant, three oxidations are taken according to proportioning
Two antimony and silicon dioxide gel are added in activation attapulgite powder, are well mixed to obtain mixed material, are added into mixed material
Enter the clear water of 3 ~ 5 times of weight, 50 ~ 60min is stirred under the conditions of 200 ~ 300r/min of rotating speed, it is fire-retardant to obtain attapulgite after standing
Agent solution；
Step（5）, to step（4）In obtained attapulgite flame retardant solution be passed through 50 ~ 60 DEG C of hot-air and seethe it, when
Between be 20 ~ 30min, carry out drying process after standing, and material is ground to form into 60 ~ 80 μm of particle, produce the attapulgite
Wood fire retardant.
Preferably, the step（3）The mass ratio of middle attapulgite powder and ethanol solution is 1：10~1：15.
Preferably, the step（3）In ultrasonically treated condition be 1000 ~ 2000W, the time be 5 ~ 30min.
Beneficial effects of the present invention：Using attapulgite as primary raw material, preparation method is simple, good flame retardation effect, for wood
The fire-retardant load medicine processing of material, it is specific as follows：
（1）, the present invention using attapulgite as raw material, through crushing and purify, by Nitrogen ion radiation treatment, then do modification
Obtain uphanging buoyancy attapulgite, suspendability is good and stably；
（2）, the present invention utilize ultrasonic technique, prepare higher suspension attapulgite alcohol suspending liquid, overcome attapulgite in ethanol
The problem of hardly possible is scattered, by adding antimony oxide, improves fire resistance；
（3）, the present invention contain higher phosphorus, nitrogen, boron, aluminium element content, for the efficient halogen-free anti-inflaming system being composited, and
It is soluble in water, fire-retardant decoction can be formulated directly into, the fire-retardant load medicine for timber is handled.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.These embodiments be merely to illustrate the present invention and without
In limitation the scope of the present invention.
Embodiment 1
A kind of attapulgite wood fire retardant, includes the raw material of following part meter：
150 parts of attapulgite；
10 parts of phosphorus-containing compound；
10 parts of amino-compound；
10 parts of boron-containing compound；
10 parts of aluminium salt；
2 parts of surfactant；
1 part of antimony oxide；
1 part of silicon dioxide gel.
Wherein, the phosphorus-containing compound is phosphoric acid, and the amino-compound is dicyandiamide.
Wherein, the boron-containing compound is boric acid, and the aluminium salt is aluminium chloride.
A kind of preparation method of attapulgite wood fire retardant is also provided in the present embodiment, comprised the following steps：
Step（1）, take attapulgite to be ground to crush to obtain attapulgite powder, 10 times of weight are poured into attapulgite powder
Clear water, the mixed liquor that high-speed stirred 5min is obtained under the conditions of rotating speed 1000r/min, stand 50min after heated, heating
Temperature is 60 DEG C, and the heat time is 20min, and the attapulgite powder after drying process is purified is carried out after heating；
Step（2）, using 10keV, 30kG nitrogen ion beam is to step（1）Attapulgite powder after the purification of middle gained is carried out
Radiation treatment, dissociation is broken up by attapulgite rod crystalline substance；
Step（3）, by step（2）Attapulgite powder after radiation treatment is added in the ethanol solution that mass concentration is 10%, with
Rotating speed 200r/min stirs 15min, then by ultrasonically treated, higher suspension attapulgite alcohol suspending liquid is obtained after standing, filters,
It is 6 to be washed to pH value, refilters, is dried to obtain activation attapulgite powder；
Step（4）, phosphorus-containing compound, amino-compound, boron-containing compound, aluminium salt, surfactant, three oxidations are taken according to proportioning
Two antimony and silicon dioxide gel are added in activation attapulgite powder, are well mixed to obtain mixed material, are added into mixed material
Enter the clear water of 3 times of weight, stirred under the conditions of rotating speed 200r/min and attapulgite flame retardant solution is obtained after 50min, standing；
Step（5）, to step（4）In obtained attapulgite flame retardant solution be passed through 50 DEG C of hot-air and seethe it, the time
For 20min, drying process is carried out after standing, and material is ground to form into 60 μm of particle, the attapulgite fire-retarding of wood is produced
Agent.
Wherein, the step（3）The mass ratio of middle attapulgite powder and ethanol solution is 1：10.
Wherein, the step（3）In ultrasonically treated condition be 1000W, the time is 5min.
Embodiment 2
A kind of attapulgite wood fire retardant, includes the raw material of following part meter：
200 parts of attapulgite；
15 parts of phosphorus-containing compound；
15 parts of amino-compound；
15 parts of boron-containing compound；
15 parts of aluminium salt；
8 parts of surfactant；
3 parts of antimony oxide；
3 parts of silicon dioxide gel.
Wherein, the phosphorus-containing compound is phosphorous acid, and the amino-compound is urea.
Wherein, the boron-containing compound is borax, and the aluminium salt is aluminum sulfate.
A kind of preparation method of attapulgite wood fire retardant is also provided in the present embodiment, comprised the following steps：
Step（1）, take attapulgite to be ground to crush to obtain attapulgite powder, 15 times of weight are poured into attapulgite powder
Clear water, the mixed liquor that high-speed stirred 10min is obtained under the conditions of rotating speed 1200r/min, stand 60min after heated, plus
Hot temperature is 85 DEG C, and the heat time is 30min, and the attapulgite powder after drying process is purified is carried out after heating；
Step（2）, using 25keV, 35kG nitrogen ion beam is to step（1）Attapulgite powder after the purification of middle gained is entered
Row radiation treatment, dissociation is broken up by attapulgite rod crystalline substance；
Step（3）, by step（2）Attapulgite powder after radiation treatment is added in the ethanol solution that mass concentration is 15%, with
Rotating speed 300r/min stirs 25min, then by ultrasonically treated, higher suspension attapulgite alcohol suspending liquid is obtained after standing, filters,
It is 8 to be washed to pH value, refilters, is dried to obtain activation attapulgite powder；
Step（4）, phosphorus-containing compound, amino-compound, boron-containing compound, aluminium salt, surfactant, three oxidations are taken according to proportioning
Two antimony and silicon dioxide gel are added in activation attapulgite powder, are well mixed to obtain mixed material, are added into mixed material
Enter the clear water of 5 times of weight, stirred under the conditions of rotating speed 300r/min and attapulgite flame retardant solution is obtained after 60min, standing；
Step（5）, to step（4）In obtained attapulgite flame retardant solution be passed through 60 DEG C of hot-air and seethe it, the time
For 30min, drying process is carried out after standing, and material is ground to form into 80 μm of particle, the attapulgite fire-retarding of wood is produced
Agent.
Wherein, the step（3）The mass ratio of middle attapulgite powder and ethanol solution is 1：15.
Wherein, the step（3）In ultrasonically treated condition be 2000W, the time is 30min.
Embodiment 3
A kind of attapulgite wood fire retardant, includes the raw material of following part meter：
175 parts of attapulgite；
12 parts of phosphorus-containing compound；
12 parts of amino-compound；
12 parts of boron-containing compound；
12 parts of aluminium salt；
5 parts of surfactant；
2 parts of antimony oxide；
2 parts of silicon dioxide gel.
Wherein, the phosphorus-containing compound is ammonium dihydrogen phosphate, and the amino-compound is urea.
Wherein, the boron-containing compound is sodium tetraborate, and the aluminium salt is aluminum nitrate.
A kind of preparation method of attapulgite wood fire retardant is also provided in the present embodiment, comprised the following steps：
Step（1）, take attapulgite to be ground to crush to obtain attapulgite powder, 12 times of weight are poured into attapulgite powder
Clear water, the mixed liquor that high-speed stirred 7min is obtained under the conditions of rotating speed 1100r/min, stand 55min after heated, heating
Temperature is 70 DEG C, and the heat time is 25min, and the attapulgite powder after drying process is purified is carried out after heating；
Step（2）, using 18keV, 32kG nitrogen ion beam is to step（1）Attapulgite powder after the purification of middle gained is carried out
Radiation treatment, dissociation is broken up by attapulgite rod crystalline substance；
Step（3）, by step（2）Attapulgite powder after radiation treatment is added in the ethanol solution that mass concentration is 12%, with
Rotating speed 250r/min stirs 20min, then by ultrasonically treated, higher suspension attapulgite alcohol suspending liquid is obtained after standing, filters,
It is 7 to be washed to pH value, refilters, is dried to obtain activation attapulgite powder；
Step（4）, phosphorus-containing compound, amino-compound, boron-containing compound, aluminium salt, surfactant, three oxidations are taken according to proportioning
Two antimony and silicon dioxide gel are added in activation attapulgite powder, are well mixed to obtain mixed material, are added into mixed material
Enter the clear water of 4 times of weight, stirred under the conditions of rotating speed 250r/min and attapulgite flame retardant solution is obtained after 55min, standing；
Step（5）, to step（4）In obtained attapulgite flame retardant solution be passed through 55 DEG C of hot-air and seethe it, the time
For 25min, drying process is carried out after standing, and material is ground to form into 70 μm of particle, the attapulgite fire-retarding of wood is produced
Agent.
Wherein, the step（3）The mass ratio of middle attapulgite powder and ethanol solution is 1：12.
Wherein, the step（3）In ultrasonically treated condition be 1500W, the time is 20min.
Embodiment 4
Use the attapulgite wood fire retardant of embodiment 1 ~ 3 to be configured to concentration for 60 ~ 80% retardant solution, take 4 piece 1000
It is progress 8 ~ 12h of pretreatment, processing in the alkali lye that 30 ~ 40 DEG C of concentration are 8 ~ 12% that × 1000 × 50mm timber floor, which is placed in temperature,
Rinsed 2 ~ 3 times with clear water after good, then 3 pieces in the plank pre-processed are immersed in respectively the retardant solution of embodiment 1 ~ 3
In 6 ~ 12h, timber floor after dipping is good infrared heating solidifies 60min, remaining 1 piece of timber floor as a control group, to this 4 blocks of wood
Floor is tested by GB (GB/T12441-2005) simulation big panel method：
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Control group | |
| Fire resistance period（min） | 92 | 96 | 95 | 10min |
Fire resistance period using the plank of attapulgite wood fire retardant of the present invention is long, and fire resistance is high.
The present invention is described in detail with reference to the foregoing embodiments, for a person skilled in the art, its according to
The technical scheme described in foregoing embodiments can so be modified, or which part technical characteristic is equally replaced
Change.Within the spirit and principles of the invention, any modifications, equivalent substitutions and improvements made etc., should be included in the present invention
Protection domain within.
Claims (9)
1. a kind of attapulgite wood fire retardant, it is characterised in that the raw material counted including following part：150 ~ 200 parts of attapulgite,
10 ~ 15 parts of phosphorus-containing compound, 10 ~ 15 parts of amino-compound, 10 ~ 15 parts of boron-containing compound, 10 ~ 15 parts of aluminium salt, surfactant 2
1 ~ 3 part of ~ 8 parts, 1 ~ 3 part of antimony oxide and silicon dioxide gel.
2. attapulgite wood fire retardant according to claim 1, it is characterised in that the raw material counted including following part：It is recessed
Convex 175 parts of rod soil, 12 parts of phosphorus-containing compound, 12 parts of amino-compound, 12 parts of boron-containing compound, 12 parts of aluminium salt, surfactant 5
2 parts of part, 2 parts of antimony oxide and silicon dioxide gel.
3. attapulgite wood fire retardant according to claim 1, it is characterised in that the phosphorus-containing compound be phosphoric acid,
Any of phosphorous acid, hypophosphorous acid, pyrophosphoric acid, APP, diammonium hydrogen phosphate, ammonium dihydrogen phosphate.
4. attapulgite wood fire retardant according to claim 1, it is characterised in that the amino-compound is dicyandiamide
Or urea.
5. attapulgite wood fire retardant according to claim 1, it is characterised in that the boron-containing compound be boric acid,
Any of borax, sodium tetraborate, borate.
6. attapulgite wood fire retardant according to claim 1, it is characterised in that the aluminium salt is aluminium chloride, sulfuric acid
Any of aluminium, aluminum nitrate.
7. a kind of preparation method of attapulgite wood fire retardant according to claim 1, it is characterised in that including as follows
Step：
Step（1）, take attapulgite to be ground to crush to obtain attapulgite powder, 10 ~ 15 weights are poured into attapulgite powder
The clear water of amount times, the mixed liquor that 5 ~ 10min of high-speed stirred is obtained under the conditions of 1000 ~ 1200r/min of rotating speed stands 50 ~ 60min
Heated afterwards, heating-up temperature is 60 ~ 85 DEG C, and the heat time is 20 ~ 30min, drying process is carried out after heating and is obtained after purification
Attapulgite powder；
Step（2）, using 10 ~ 25keV, 30 ~ 35kG nitrogen ion beam is to step（1）Attapulgite powder after the purification of middle gained
End carries out radiation treatment, and attapulgite rod crystalline substance is broken up into dissociation；
Step（3）, by step（2）Attapulgite powder after radiation treatment adds the ethanol solution that mass concentration is 10 ~ 15%
In, 15 ~ 25min is stirred with 200 ~ 300r/min of rotating speed, then by ultrasonically treated, higher suspension attapulgite ethanol is obtained after standing
Suspension, filtering, it is 6 ~ 8 to be washed to pH value, refilters, is dried to obtain activation attapulgite powder；
Step（4）, phosphorus-containing compound, amino-compound, boron-containing compound, aluminium salt, surfactant, three oxidations are taken according to proportioning
Two antimony and silicon dioxide gel are added in activation attapulgite powder, are well mixed to obtain mixed material, are added into mixed material
Enter the clear water of 3 ~ 5 times of weight, 50 ~ 60min is stirred under the conditions of 200 ~ 300r/min of rotating speed, it is fire-retardant to obtain attapulgite after standing
Agent solution；
Step（5）, to step（4）In obtained attapulgite flame retardant solution be passed through 50 ~ 60 DEG C of hot-air and seethe it, when
Between be 20 ~ 30min, carry out drying process after standing, and material is ground to form into 60 ~ 80 μm of particle, produce the attapulgite
Wood fire retardant.
8. the preparation method of attapulgite wood fire retardant according to claim 7, it is characterised in that the step（3）
The mass ratio of middle attapulgite powder and ethanol solution is 1：10~1：15.
9. the preparation method of attapulgite wood fire retardant according to claim 7, it is characterised in that the step（3）
In ultrasonically treated condition be 1000 ~ 2000W, the time be 5 ~ 30min.
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Cited By (5)
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| CN108748503A (en) * | 2018-06-12 | 2018-11-06 | 阜南县创发工艺品有限公司 | A method of extending the fast growing wood outdoor application time limit |
| CN109233310A (en) * | 2018-09-11 | 2019-01-18 | 界首永恩机电科技有限公司 | A kind of attapulgite and preparation method thereof for modifying plastics |
| CN114606049A (en) * | 2022-03-21 | 2022-06-10 | 温州尚脉生物科技有限公司 | Preparation method of high-quality olive oil |
| CN115340773A (en) * | 2022-06-27 | 2022-11-15 | 安徽爱瑞德新材料有限公司 | Preparation method of high-strength flame-retardant wood-plastic composite material |
| CN115340773B (en) * | 2022-06-27 | 2024-05-14 | 安徽爱瑞德新材料有限公司 | Preparation method of high-strength flame-retardant wood-plastic composite material |
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| CN108748503A (en) * | 2018-06-12 | 2018-11-06 | 阜南县创发工艺品有限公司 | A method of extending the fast growing wood outdoor application time limit |
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| CN115340773A (en) * | 2022-06-27 | 2022-11-15 | 安徽爱瑞德新材料有限公司 | Preparation method of high-strength flame-retardant wood-plastic composite material |
| CN115340773B (en) * | 2022-06-27 | 2024-05-14 | 安徽爱瑞德新材料有限公司 | Preparation method of high-strength flame-retardant wood-plastic composite material |
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Application publication date: 20170718 |