CN115637078B - Preparation method of flame retardant with controllable thickness of expanded carbon layer and flame retardant wood - Google Patents
Preparation method of flame retardant with controllable thickness of expanded carbon layer and flame retardant wood Download PDFInfo
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- CN115637078B CN115637078B CN202211358671.6A CN202211358671A CN115637078B CN 115637078 B CN115637078 B CN 115637078B CN 202211358671 A CN202211358671 A CN 202211358671A CN 115637078 B CN115637078 B CN 115637078B
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 85
- 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 title claims abstract description 81
- 239000002023 wood Substances 0.000 title claims abstract description 42
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 235000002949 phytic acid Nutrition 0.000 claims abstract description 62
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims abstract description 60
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000004202 carbamide Substances 0.000 claims abstract description 36
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229940068041 phytic acid Drugs 0.000 claims abstract description 32
- 239000000467 phytic acid Substances 0.000 claims abstract description 32
- 239000007787 solid Substances 0.000 claims abstract description 30
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 28
- 229920002472 Starch Polymers 0.000 claims abstract description 26
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000008107 starch Substances 0.000 claims abstract description 23
- 235000019698 starch Nutrition 0.000 claims abstract description 23
- 239000000543 intermediate Substances 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 229960000583 acetic acid Drugs 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010992 reflux Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 239000002131 composite material Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 229920001592 potato starch Polymers 0.000 claims description 7
- 229920002261 Corn starch Polymers 0.000 claims description 3
- 240000003183 Manihot esculenta Species 0.000 claims description 3
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 claims description 3
- 239000008120 corn starch Substances 0.000 claims description 3
- 229940100445 wheat starch Drugs 0.000 claims description 3
- 230000001276 controlling effect Effects 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 230000008014 freezing Effects 0.000 abstract 1
- 238000007710 freezing Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 23
- 239000000779 smoke Substances 0.000 description 14
- 241000219000 Populus Species 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 9
- 238000000576 coating method Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 238000002485 combustion reaction Methods 0.000 description 4
- 239000003973 paint Substances 0.000 description 4
- 239000004566 building material Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000003517 fume Substances 0.000 description 3
- 239000003345 natural gas Substances 0.000 description 3
- -1 ammonium phytates Chemical class 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 230000026030 halogenation Effects 0.000 description 2
- 238000005658 halogenation reaction Methods 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 231100000053 low toxicity Toxicity 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000007480 spreading Effects 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
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- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Abstract
The invention belongs to the technical field of wood processing, and particularly relates to a flame retardant with a thickness-controllable expanded carbon layer and a preparation method of flame retardant wood, wherein the preparation of the flame retardant comprises the following steps: placing phytic acid and urea into a reaction container, and heating, condensing and refluxing to obtain oily liquid; freezing the oily liquid in ultralow temperature equipment; drying by a freeze dryer to obtain a solid intermediate; adding the solid intermediate, starch and glacial acetic acid into pure water, heating and stirring to obtain the required flame retardant; the flame retardant is coated on raw wood, and the flame retardant wood can be prepared through drying in the shade, drying and balancing moisture. The invention adopts phytic acid and urea as raw materials to obtain ammonium phytate with different reaction degrees; the purposes of regulating and controlling the thickness of the starch-based flame-retardant intumescent carbon layer are achieved by utilizing the different proportions of phytic acid, ammonium phytate and urea, and the application of the starch-based intumescent flame retardant as a wood flame retardant is expanded.
Description
Technical Field
The invention belongs to the technical field of wood processing, and particularly relates to a flame retardant with a thickness-controllable expanded carbon layer and a preparation method of flame retardant wood.
Background
Wood plays an important role in the life of people as a natural degradable environment-friendly material. But its application is greatly limited due to its flammability. Therefore, the excellent performance of the wood is exerted, and the modified wood is subjected to modification treatment, so that the flame retardant performance of the wood is improved, the application range of the wood is widened, and the modified wood is an important way for saving wood resources and meeting the needs of various functions of people in life.
With the increasing demand for flame retardance and the increasing environmental awareness in recent years, the non-halogenation, smoke suppression and attenuation of flame retardants have become a leading topic in the current and future research fields of flame retardants. Compared with the traditional flame retardant, the novel environment-friendly flame retardant has the serious defects of large addition amount, large smoke generation amount, toxic and corrosive gas generation and the like. Intumescent flame retardants are novel composite flame retardants which are widely focused in the field of flame retardance in China in recent years. The flame retardant has unique flame retardant mechanism and the characteristics of no halogen, low smoke and low toxicity, and is an important way for no halogenation of the flame retardant. The expansion flame-retardant system forms a compact porous foam carbon layer on the surface of the material during combustion due to the synergistic effect of an acid source, a carbon source and an air source. The flame-retardant composite material can prevent further degradation of the inner-layer high polymer and release of combustible materials to the surface, and can prevent heat sources from transmitting to the high polymer and isolating oxygen sources, so that flame is prevented from spreading and spreading. The intumescent flame retardant has excellent flame retardant property, has the advantages of no halogen, low smoke, low toxicity, molten drop prevention and no corrosive gas, accords with the development direction of the future flame retardant, and has very broad development prospect.
However, the existing intumescent flame retardant still has the defects when being used as a wood flame retardant, and the thickness of an intumescent carbon layer cannot be effectively controlled, so that the application of the intumescent carbon layer is limited. Accordingly, there is a need for providing an intumescent char layer thickness controllable flame retardant and a method for preparing flame retardant wood using the same.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a flame retardant with a controllable thickness of an expanded carbon layer and a preparation method of flame retardant wood.
In order to achieve the technical purpose and the technical effect, the invention is realized by the following technical scheme:
the invention provides a flame retardant with a controllable thickness of an expanded carbon layer, which comprises the following steps:
1) Placing phytic acid and urea into a reaction container according to a certain molar ratio, heating, condensing and refluxing for 4-8 hours at the temperature of 90-130 ℃ to obtain oily liquid;
2) The obtained oily liquid is put into ultralow temperature equipment and frozen for 12 to 48 hours at the temperature of minus 80 ℃; then drying for 12-48 hours at the temperature of minus 50 ℃ by using a freeze dryer to obtain a solid intermediate;
3) Adding the obtained solid intermediate, starch and glacial acetic acid into proper amount of pure water according to a certain mass ratio, heating and stirring for 5-20 min at 85-95 ℃ to obtain the required flame retardant.
Further, the molar ratio of the phytic acid to the urea is 1:x, wherein x=3-20;
when x=6, the solid intermediate obtained in step 2) is ammonium phytate solid;
when x is less than 6, the solid intermediate obtained in the step 2) is a phytic acid/ammonium phytate composite solid;
when x >6, the solid intermediate obtained in step 2) is a urea/ammonium phytate complex solid.
Further, in the step 1), the condensate reflux is heated at 120 ℃ for 6 hours.
Further, in the step 2), the obtained oily liquid is put into ultra-low temperature equipment and frozen for 24 hours at the temperature of-80 ℃.
Further, in step 2), the mixture was dried at-50℃for 24 hours using a freeze dryer.
Further, in the step 3), the mixture is heated and stirred for 5 to 20 minutes at a temperature of between 85 and 95 ℃.
Further, in the step 3), the starch is at least one of potato starch, corn starch, tapioca starch and wheat starch.
Further, in the step 3), the mass ratio of the solid intermediate to the starch to the glacial acetic acid is 5-15:5-15:1.
Further, the mass ratio of the solid intermediate to the starch to the glacial acetic acid is 10:10:1.
The invention also provides a method for preparing flame-retardant wood by using the flame retardant with the thickness controllable expanded carbon layer, which comprises the following steps:
s1, firstly, the flame retardant is mixed according to the proportion of 0.20-0.30 g/cm 2 Smearing the raw wood board;
s2, drying the raw material wood board coated with the flame retardant in the shade for 2-4 hours, and drying at the temperature of 40 ℃ to obtain a dried wood board;
s3, placing the obtained dried wood board in a constant temperature and humidity box, and balancing the moisture at the temperature of 22 ℃ and under the humidity condition of 65%, wherein the balancing time is more than or equal to 80h.
The beneficial effects of the invention are as follows:
the invention adopts phytic acid and urea as raw materials to obtain ammonium phytate with different reaction degrees, wherein the phytic acid is used as an acid source, the ammonium phytate is used as an acid source and a gas source, and the urea is used as a gas source; the purposes of regulating and controlling the thickness of the starch-based flame-retardant intumescent carbon layer are achieved by utilizing the different proportions of phytic acid, ammonium phytate and urea, and the application of the starch-based intumescent flame retardant as a wood flame retardant is expanded.
Of course, it is not necessary for any one product to practice the invention to achieve all of the advantages set forth above at the same time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an infrared plot of each group of ammonium phytates in examples 1-7;
FIG. 2 is a graph showing the smoke density level distribution of comparative examples 1-2 and examples 1-7;
FIG. 3 is a schematic diagram of the reaction of phytic acid and urea.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a flame retardant with a controllable thickness of an expanded carbon layer, which comprises the following steps:
1) Placing phytic acid and urea into a reaction container according to a certain molar ratio, heating, condensing and refluxing for 4-8 hours at the temperature of 90-130 ℃ to obtain oily liquid;
2) The obtained oily liquid is put into ultralow temperature equipment and frozen for 12 to 48 hours at the temperature of minus 80 ℃; then drying for 12-48 hours at the temperature of minus 50 ℃ by using a freeze dryer to obtain a solid intermediate;
3) Adding the obtained solid intermediate, starch and glacial acetic acid into proper amount of pure water according to a certain mass ratio, heating and stirring for 5-20 min at 85-95 ℃ to obtain the required flame retardant.
In the invention, the molar ratio of the phytic acid to the urea is 1:x, wherein x=3-20;
when x=6, the solid intermediate obtained in step 2) is ammonium phytate solid;
when x is less than 6, the solid intermediate obtained in the step 2) is a phytic acid/ammonium phytate composite solid;
when x >6, the solid intermediate obtained in step 2) is a urea/ammonium phytate complex solid.
In the invention, the starch is at least one of potato starch, corn starch, tapioca starch and wheat starch.
In the invention, the mass ratio of the solid intermediate to the starch to the glacial acetic acid is 5-15:5-15:1.
The method for preparing the flame-retardant wood by using the flame retardant with the thickness of the expanded carbon layer controllable comprises the following steps:
s1, firstly, the flame retardant is mixed according to the proportion of 0.20-0.30 g/cm 2 (wherein the flame retardant agentThe effective component coating amount is 0.035-0.052 g/cm 2 ) Smearing the raw wood board;
s2, drying the raw material wood board coated with the flame retardant in the shade for 2-4 hours, and drying at the temperature of 40 ℃ to obtain a dried wood board;
s3, placing the obtained dried wood board in a constant temperature and humidity box, and balancing the moisture at the temperature of 22 ℃ and under the humidity condition of 65%, wherein the balancing time is more than or equal to 80h.
The invention adopts phytic acid and urea as raw materials to obtain the ammonium phytate with different reaction degrees, the reaction mechanism is shown in figure 3, wherein the phytic acid is used as an acid source, the ammonium phytate is used as an acid source and a gas source, and the urea is used as a gas source.
The specific embodiment of the invention is as follows:
example 1
1) Preparation of phytic acid/ammonium phytate composite flame retardant
The phytic acid and the urea are put into a three-necked flask according to the mol ratio of 1:3, and are heated, condensed and refluxed for 6 hours at 120 ℃ to obtain pale yellow oily liquid. Then the mixture is put into an ultralow temperature refrigerator with the temperature of minus 80 ℃ to be frozen for 24 hours. And then drying for 24 hours at minus 50 ℃ by using a freeze dryer to obtain the phytic acid/ammonium phytate composite flame retardant in a white solid state, wherein the mole ratio of the phytic acid to the ammonium phytate is 1:1.
2) Preparation of flame retardant coating
10g of potato starch, 10g of phytic acid/ammonium phytate composite flame retardant solid and 1g of glacial acetic acid are dissolved in 100g of pure water, and the mixture is heated and stirred at 90 ℃ for 10min to obtain the flame retardant coating.
3) Flame retardant wood preparation
The intumescent flame retardant obtained above was mixed according to a ratio of 0.25g/cm 2 The paint is smeared on poplar samples, and the specifications of the samples are 100mm long by 50mm wide by 5mm thick. The smeared samples were dried in the shade for 3 hours in a fume hood, then dried in a forced air oven at 40℃and then equilibrated for 88 hours in a constant temperature and humidity oven at 22℃and 65% humidity.
Example 2
1) Preparation of ammonium phytate flame retardant
The phytic acid and the urea are put into a three-necked flask according to the mol ratio of 1:6, and are heated, condensed and refluxed for 6 hours at 120 ℃ to obtain pale yellow oily liquid. Then the mixture is put into an ultralow temperature refrigerator with the temperature of minus 80 ℃ to be frozen for 24 hours. And then drying for 24 hours at minus 50 ℃ by using a freeze dryer to obtain white ammonium phytate.
2) Preparation of flame retardant coating
10g of potato starch, 10g of ammonium phytate flame retardant solid and 1g of glacial acetic acid are dissolved in 100g of pure water, and the mixture is heated and stirred at 90 ℃ for 10min to obtain the flame retardant coating.
3) Flame retardant wood preparation
The intumescent flame retardant obtained above was mixed according to a ratio of 0.25g/cm 2 (wherein the effective application amount of the flame retardant is 0.043 g/cm) 2 ) The paint is smeared on poplar samples, and the specifications of the samples are 100mm long by 50mm wide by 5mm thick. The smeared samples were dried in the shade for 3 hours in a fume hood, then dried in a forced air oven at 40℃and then equilibrated for 88 hours in a constant temperature and humidity oven at 22℃and 65% humidity.
Example 3
1) Preparation of urea/ammonium phytate composite flame retardant
The phytic acid and the urea are put into a three-necked flask according to the mol ratio of 1:9, and are heated, condensed and refluxed for 6 hours at 120 ℃ to obtain pale yellow oily liquid. Then the mixture is put into an ultralow temperature refrigerator with the temperature of minus 80 ℃ to be frozen for 24 hours. And then drying for 24 hours at minus 50 ℃ by using a freeze dryer to obtain the urea/ammonium phytate composite flame retardant in a white solid state.
2) Preparation of flame retardant coating
10g of potato starch, 10g of urea/ammonium phytate composite flame retardant solid and 1g of glacial acetic acid are dissolved in 100g of pure water, and the mixture is heated and stirred at 90 ℃ for 10min to obtain the flame retardant coating.
3) Flame retardant wood preparation
The intumescent flame retardant obtained above was mixed according to a ratio of 0.25g/cm 2 (wherein the effective application amount of the flame retardant is 0.043 g/cm) 2 ) The paint is smeared on poplar samples, and the specifications of the samples are 100mm long by 50mm wide by 5mm thick. The smeared samples were dried in the shade for 3 hours in a fume hood, then dried in a forced air oven at 40℃and then equilibrated for 88 hours in a constant temperature and humidity oven at 22℃and 65% humidity.
Example 4
This example is essentially the same as example 3, except that the molar ratio of phytic acid to urea is 1:12.
Example 5
This example is essentially the same as example 3, except that the molar ratio of phytic acid to urea is 1:15.
Example 6
This example is essentially the same as example 3, except that the molar ratio of phytic acid to urea is 1:18.
Example 7
This example is essentially the same as example 3, except that the molar ratio of phytic acid to urea is 1:20.
Comparative example 1
The specification of the poplar material is 100mm long by 50mm wide by 5mm thick for untreated poplar material.
Comparative example 2
Dissolving 10g of potato starch and 1g of acetic acid in 100g of pure water, stirring and heating at 90 ℃ for 10min to obtain starch coating according to 0.25g/cm 2 The paint is uniformly smeared on the surface of a poplar sample, and the specification of the sample is 100mm long by 50mm wide by 5mm thick.
Fourier infrared testing
The chemical structure of the ammonium phytate starch coating was characterized using a fourier transform infrared spectrometer. The sample preparation method is KBr tabletting method, and the wave number scanning range is 400-4000cm -1 The number of scans was 32, the resolution was 4cm -1 。
The infrared curves of each group of ammonium phytates are shown in FIG. 1, from which it can be seen that at 1450cm -1 And 3210cm -1 The stronger absorption peak is formed by NH 4+ Is caused by bending and stretching vibration at 1050cm at the same time -1 、965cm -1 The characteristic peaks of P-O, P =o appear respectively, and the experimental phenomenon can prove that PA and Urea react successfully to generate ammonium phytate.
Meaning of symbols in the drawings: 1-3 represents that the mole ratio of the phytic acid and the urea serving as reaction raw materials is 1:3,1-6, 1-9, 1-12, 1-15, 1-18 and 1-20 are similar.
Thickness test of expanded carbon layer
The experimental equipment adopts a JL-JCF-3 (Nanjing Torpedo) building material smoke density tester, and under the natural gas pressure of 0.2MPa, an open fire test is carried out on a wood board with the thickness of 100mm multiplied by 50mm multiplied by 10mm, and the test results are shown in Table 1:
TABLE 1 thickness of expanded carbon layers
With the increase of the proportion of urea, the thickness of the carbon layer tends to be increased and then reduced, and the main reason is that the phytic acid content in the system is reduced to generate a large amount of ammonium phytate, and the phytic acid catalyzes the carbon source to form carbon, and simultaneously, the urea and the ammonium phytate are decomposed to generate a large amount of gas, so that the thickness of the carbon layer is increased. As the urea ratio is greater than 12, the thickness of the carbon layer gradually decreases, mainly because of the presence of a large amount of urea in the system, and when heated, a large amount of gas is evolved to break the carbon layer, resulting in a decrease in the thickness of the carbon layer.
Limiting oxygen index test
According to GB/T2406-1993, a fully automatic oxygen index tester of JL-JF-5 (Nanjing Lei) is adopted to test the sample according to the GB/T2406-93 standard, and the size of the sample is 130mm multiplied by 6.5mm multiplied by 3mm. Each sample was tested 5 times and the test results are shown in table 2:
TABLE 2 oxygen index distribution
As can be seen from Table 2, the flame retardant treated poplar samples, except 1-3 groups, have oxygen index of more than 60%, which is sufficient to demonstrate that the intumescent flame retardant has good flame retardant effect.
Smoke density performance test
The experimental equipment adopts a JL-JCF-3 (Nanjing Bright mine) building material smoke density tester to test the smoke density under the condition that the natural gas pressure is 0.2 MPa. Each group of samples was tested 5 times to average.
The smoke density grade distribution is shown in figure 2, and it can be seen from the figure that the smoke density grade of the starch treatment group is far greater than that of the poplar wood sample, and the smoke density grades of the other groups except 1-3 groups are all greater than that of the poplar wood sample but smaller than that of the starch treatment group, because the expansion height of the carbon layers of 1-3 groups is not high and the cracking condition is less, and the carbon layers of the other treatment groups are more compact and more expanded than those of 1-3 groups, but cracks are generated in heating, so that a great amount of smoke is emitted from the wood yin.
Symbol meaning: 1-3 represents that the mole ratio of the phytic acid and the urea serving as reaction raw materials is 1:3,1-6, 1-9, 1-12, 1-15, 1-18 and 1-20 are similar.
Combustion quality test
The experimental equipment adopts a JL-JCF-3 (Nanjing Torpedo) building material smoke density tester to burn for 3min under the pressure of natural gas of 0.2MPa, and the result is shown in Table 3:
TABLE 3 mass change before and after combustion
As can be seen from the table, the poplar-like and starch treated group lost a significant amount of mass before and after combustion and had been depleted. The loss of less mass is enough to indicate that the flame retardant effect is excellent through the flame retardant coating layer, and the loss mass is in a trend of rising and then falling along with the increase of the urea content, which is the same as the thickness of the carbon layer.
The preferred embodiments of the invention disclosed above are merely helpful in explaining the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (6)
1. The method for preparing the flame-retardant wood by using the flame retardant with the thickness of the expanded carbon layer is characterized by comprising the following steps of:
s1, firstly, the thickness-controllable flame retardant of the expanded carbon layer is prepared according to the proportion of 0.20-0.30 g/cm 2 Smearing the raw wood board;
the preparation process of the flame retardant with the controllable thickness of the expanded carbon layer comprises the following steps:
1) Placing phytic acid and urea into a reaction container according to a certain molar ratio, heating, condensing and refluxing for 4-8 hours at the temperature of 90-130 ℃ to obtain oily liquid;
the molar ratio of the phytic acid to the urea is 1:x, wherein x=12-20;
2) The obtained oily liquid is put into ultralow temperature equipment and frozen for 12 to 48 hours at the temperature of minus 80 ℃; drying for 12-48 h at-50 ℃ by using a freeze dryer to obtain a solid intermediate which is urea/ammonium phytate composite solid;
3) Adding the obtained solid intermediate, starch and glacial acetic acid into proper amount of pure water according to the mass ratio of 5-15:5-15:1, heating and stirring for 5-20 min at the temperature of 85-95 ℃ to obtain the expansion carbon layer thickness-controllable flame retardant;
s2, drying the raw material wood board coated with the flame retardant in the shade for 2-4 hours, and drying at the temperature of 40 ℃ to obtain a dried wood board;
s3, placing the obtained dried wood board in a constant temperature and humidity box, and balancing the moisture at the temperature of 22 ℃ and under the humidity condition of 65%, wherein the balancing time is more than or equal to 80h.
2. The method according to claim 1, characterized in that: in step 1), the mixture is heated, condensed and refluxed at 120 ℃ for 6 hours.
3. The method according to claim 1, characterized in that: in the step 2), the obtained oily liquid is put into ultralow temperature equipment and frozen for 24 hours at the temperature of minus 80 ℃.
4. The method according to claim 1, characterized in that: in step 2), the mixture was dried at-50℃for 24 hours using a freeze dryer.
5. The method according to claim 1, characterized in that: in the step 3), the starch is at least one of potato starch, corn starch, tapioca starch and wheat starch.
6. The method according to claim 1, characterized in that: the mass ratio of the solid intermediate to the starch to the glacial acetic acid is 10:10:1.
Priority Applications (1)
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