CN114015116A - Preparation method of aluminum hydroxide surface modified expandable graphite flame retardant and method for preparing flame-retardant polyurethane foam plastic by using same - Google Patents
Preparation method of aluminum hydroxide surface modified expandable graphite flame retardant and method for preparing flame-retardant polyurethane foam plastic by using same Download PDFInfo
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Abstract
A preparation method of an aluminum hydroxide surface modified expandable graphite flame retardant and a method for preparing flame-retardant polyurethane foam plastic by using the same belong to the field of flame-retardant materials, and particularly relate to a preparation method of a modified expandable graphite flame retardant and a method for preparing flame-retardant polyurethane foam plastic by using the same. The invention aims to solve the problems that the existing aluminum hydroxide flame retardant is more uniformly dispersed in polyurethane foam and the existing polyurethane foam plastic has poor mechanical properties. The preparation method comprises the following steps: the catalyst is prepared from sodium hydroxide, aluminum hydroxide and expandable graphite by a hydrothermal method. The method for preparing the flame-retardant polyurethane foam plastic comprises the following steps: firstly, weighing; secondly, mixing; and thirdly, curing. The advantages are that: the limiting oxygen index can be improved to 28.5%; the compressive strength is improved to 0.162MPa, and the closed porosity is improved. The invention is mainly used for preparing the aluminum hydroxide surface modified expandable graphite flame retardant and the flame-retardant polyurethane foam plastic.
Description
Technical Field
The invention belongs to the field of flame-retardant materials, and particularly relates to a preparation method of a modified expandable graphite flame retardant and a method for preparing flame-retardant polyurethane foam plastic by using the modified expandable graphite flame retardant.
Background
At present, the building energy consumption of China accounts for 1/3 of the total social energy consumption, and the building energy saving still increases at a speed of 1% per year, so that the building energy saving becomes a basic national policy of China. The total area of buildings in China is about 400 hundred million square meters, and high-energy-consumption buildings account for more than 95 percent, which is the main reason for high energy consumption of buildings in China. Heat transfer through walls, pipelines, roofs and the like is a main way for energy consumption of buildings, and the heat conductivity coefficient of the hard polyurethane foam plastic is the lowest of all organic heat-insulating materials, so that the hard polyurethane foam plastic has excellent heat-insulating and heat-preserving performance. Although polyurethane foam has excellent heat insulation performance, the oxygen index of hard foam which is not subjected to flame retardant treatment is only 16-18%, the hard foam is extremely easy to burn, and a large amount of toxic smoke is released in the burning process, so that the life and property safety of people is greatly threatened. Therefore, the research on the preparation of the flame-retardant rigid polyurethane foam plastic has very important practical significance.
In order to improve flame retardancy of polyurethane foams, various flame retardants are generally added to the polyurethane foams. Common flame retardants are classified into additive flame retardants and reactive flame retardants, and additive flame retardants are classified into organic flame retardants and inorganic flame retardants. Among inorganic flame retardants, aluminum hydroxide, magnesium hydroxide, montmorillonite, expandable graphite, red phosphorus, and the like are used in many practical applications. The aluminum hydroxide serving as a flame retardant can not only resist flame, but also prevent smoke generation, does not generate dropping matters and toxic gas; the expandable graphite has the characteristics of no toxicity, no pollution and the like, but in practical application, the aluminum hydroxide and the expandable graphite flame retardant are compounded and used together only by mechanical mixing, and the maximum flame retardant property cannot be exerted.
Disclosure of Invention
The invention aims to solve the problems that the existing aluminum hydroxide flame retardant is more uniformly dispersed in polyurethane foam and the existing polyurethane foam plastic has poor mechanical property, and provides a preparation method of an aluminum hydroxide surface modified expandable graphite flame retardant and a method for preparing flame-retardant polyurethane foam plastic by using the same.
The preparation method of the aluminum hydroxide surface modified expandable graphite flame retardant comprises the following steps: the expandable graphite flame retardant with the modified aluminum hydroxide surface is prepared by taking sodium hydroxide, aluminum hydroxide and expandable graphite as raw materials and adopting a hydrothermal method.
The method for preparing the flame-retardant polyurethane foam plastic by using the aluminum hydroxide surface modified expandable graphite flame retardant is specifically completed according to the following steps:
firstly, weighing: weighing 100 parts of polyether polyol, 0.8-1.2 parts of deionized water, 8-12 parts of n-pentane, 0.4-0.8 part of triethanolamine, 0.3-0.5 part of dibutyltin dilaurate, 6-10 parts of silicone oil, 5-20 parts of aluminum hydroxide surface modified expandable graphite flame retardant, 5-15 parts of dioctyl adipate and 130-170 parts of isocyanate according to parts by weight;
secondly, mixing: stirring and mixing 100 parts of polyether polyol, 0.8-1.2 parts of deionized water, 8-12 parts of n-pentane, 0.4-0.8 part of triethanolamine, 0.3-0.5 part of dibutyltin dilaurate, 6-10 parts of silicone oil, 5-20 parts of aluminum hydroxide surface modified expandable graphite flame retardant and 5-15 parts of dioctyl adipate weighed in the first step to obtain a mixture;
thirdly, curing: and (3) adding 130-170 parts of isocyanate weighed in the step (I) into the mixture obtained in the step (II), firstly stirring for 7-13 s, then pouring into a mold, standing until the foaming is complete, then transferring into an oven, and curing for 1.7-2.3 h at the temperature of 60-80 ℃ to obtain the flame-retardant polyurethane foam plastic.
The invention has the advantages that:
compared with the traditional aluminum hydroxide flame retardant, the aluminum hydroxide surface-modified expandable graphite flame retardant is dispersed in polyurethane foam more uniformly, so that the flame-retardant polyurethane foam has a better flame-retardant effect, and the limited oxygen index can be improved to 28.5%;
the aluminum hydroxide surface modified expandable graphite flame retardant reduces the grain size of aluminum hydroxide, improves the mechanical property of polyurethane foam plastic by matching with a plasticizer, improves the compression strength to 0.162MPa, and reaches the II-level standard of the compression strength;
thirdly, adding an aluminum hydroxide surface modified expandable graphite flame retardant and a plasticizer into the flame-retardant polyurethane foam plastic to improve the closed cell rate of polyurethane;
according to different requirements of the flame-retardant polyurethane foam plastic, the flame-retardant polyurethane foam plastic without flame-retardant performance is prepared by changing the addition amount of the aluminum hydroxide surface modified expandable graphite flame retardant, so that the cost is saved;
the preparation method for the aluminum hydroxide surface modified expandable graphite flame retardant and the flame-retardant polyurethane foam plastic has the advantages of simple process equipment, simple steps, safe preparation process, no harmful substances in raw materials and high industrial production value.
The expandable graphite flame retardant and the flame-retardant polyurethane foam plastic with the modified aluminum hydroxide surface prepared by the invention can be widely applied to the field of buildings.
Drawings
FIG. 1 is a scanning electron microscope image of an aluminum hydroxide surface-modified expandable graphite flame retardant obtained in example 1;
FIG. 2 is an XRD pattern, wherein A shows the XRD pattern of the aluminum hydroxide surface-modified expandable graphite flame retardant obtained in example 1, and B shows the XRD pattern of the aluminum hydroxide surface-modified expandable graphite flame retardant obtained in example 2; c represents the XRD pattern of the aluminum hydroxide surface-modified expandable graphite flame retardant obtained in example 3; d represents the XRD pattern of expandable graphite;
FIG. 3 is a schematic structural diagram of a strip-shaped test piece.
Detailed Description
The first embodiment is as follows: the embodiment is a preparation method of an aluminum hydroxide surface modified expandable graphite flame retardant, which is specifically completed by the following steps: the expandable graphite flame retardant with the modified aluminum hydroxide surface is prepared by taking sodium hydroxide, aluminum hydroxide and expandable graphite as raw materials and adopting a hydrothermal method.
The second embodiment is as follows: the present embodiment differs from the first embodiment in that: the mass fraction of the aluminum hydroxide in the aluminum hydroxide surface modified expandable graphite flame retardant is 30-45%. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the hydrothermal method comprises the following specific operation processes: placing expandable graphite and aluminum hydroxide into a reaction kettle, adding a sodium hydroxide solution with the pH value of 11, uniformly stirring, covering the reaction kettle, heating to 200-220 ℃, reacting at the temperature of 200-220 ℃ for 1.5-2.5 h, cooling to room temperature to obtain a solid-liquid mixture, and sequentially filtering, washing and vacuum drying to obtain the aluminum hydroxide surface modified expandable graphite flame retardant. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is as follows: the mass ratio of the expandable graphite to the aluminum hydroxide is 1 (1-1.2); the volume ratio of the mass of the expandable graphite to the sodium hydroxide solution with the pH value of 11 is 1g (9-12) mL. The others are the same as the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the filtration is specifically performed as follows: and filtering the solid-liquid mixture by using filter paper to obtain a filter cake. The rest is the same as the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is as follows: the washing operation is as follows: and washing the filter cake with deionized water for 3-5 times to obtain a washed solid, wherein the volume ratio of the mass of the filter cake to the volume of the deionized water in a single washing is 1g (30-50) mL. The rest is the same as the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the vacuum drying operation is as follows: and (3) putting the washed solid in a vacuum drying oven, and carrying out vacuum drying for 4-6 h at the temperature of 60-80 ℃ to obtain the aluminum hydroxide surface modified expandable graphite flame retardant. The rest is the same as the first to sixth embodiments.
The specific implementation mode is eight: the embodiment is a method for preparing flame-retardant polyurethane foam plastic by using an aluminum hydroxide surface modified expandable graphite flame retardant, which is specifically completed according to the following steps:
firstly, weighing: weighing 100 parts of polyether polyol, 0.8-1.2 parts of deionized water, 8-12 parts of n-pentane, 0.4-0.8 part of triethanolamine, 0.3-0.5 part of dibutyltin dilaurate, 6-10 parts of silicone oil, 5-20 parts of aluminum hydroxide surface modified expandable graphite flame retardant, 5-15 parts of dioctyl adipate and 130-170 parts of isocyanate according to parts by weight;
secondly, mixing: stirring and mixing 100 parts of polyether polyol, 0.8-1.2 parts of deionized water, 8-12 parts of n-pentane, 0.4-0.8 part of triethanolamine, 0.3-0.5 part of dibutyltin dilaurate, 6-10 parts of silicone oil, 5-20 parts of aluminum hydroxide surface modified expandable graphite flame retardant and 5-15 parts of dioctyl adipate weighed in the first step to obtain a mixture;
thirdly, curing: and (3) adding 130-170 parts of isocyanate weighed in the step (I) into the mixture obtained in the step (II), firstly stirring for 7-13 s, then pouring into a mold, standing until the foaming is complete, then transferring into an oven, and curing for 1.7-2.3 h at the temperature of 60-80 ℃ to obtain the flame-retardant polyurethane foam plastic.
The specific implementation method nine: the present embodiment is different from the eighth embodiment in that: in the first step, 100 parts of polyether polyol, 1 part of deionized water, 10 parts of n-pentane, 0.6 part of triethanolamine, 0.4 part of dibutyltin dilaurate, 8 parts of silicone oil, 5-20 parts of aluminum hydroxide surface-modified expandable graphite flame retardant, 5-15 parts of dioctyl adipate and 150 parts of isocyanate are weighed according to parts by weight. The rest is the same as the embodiment eight.
The detailed implementation mode is ten: the eighth embodiment is different from the ninth embodiment in that: the stirring and mixing operation in the second step is as follows: stirring and mixing for 4-10 min by a mechanical stirrer. The others are the same as the embodiments eight or nine.
The invention is not limited to the above embodiments, and one or a combination of several embodiments may also achieve the object of the invention.
The following tests are adopted to verify the effect of the invention:
example 1: the preparation method of the aluminum hydroxide surface modified expandable graphite flame retardant comprises the following steps:
adding 1.0g of 80-mesh expandable graphite and 2.2g of aluminum hydroxide into a reaction kettle, adding 10ml of sodium hydroxide solution with the pH value of 11, uniformly stirring, covering the reaction kettle, heating to 210 ℃, reacting for 2 hours at the temperature of 210 ℃, and cooling to room temperature to obtain a solid-liquid mixture; filtering the solid-liquid mixture by using filter paper to obtain a filter cake; washing the filter cake with deionized water for 4 times to obtain a washed solid; the volume ratio of the mass of the filter cake to the deionized water in single washing is 1g:40 mL; and (3) putting the washed solid in a vacuum drying oven, and carrying out vacuum drying for 4h at the temperature of 70 ℃ to obtain the aluminum hydroxide surface modified expandable graphite flame retardant.
The mass fraction of aluminum hydroxide in the aluminum hydroxide surface-modified expandable graphite flame retardant described in example 1 was 38%.
FIG. 1 is a scanning electron microscope image of an aluminum hydroxide surface-modified expandable graphite flame retardant obtained in example 1; as is apparent from fig. 1, aluminum hydroxide powder is effectively attached to the surface of expandable graphite.
Example 2: the present embodiment is different from embodiment 1 in that: the pH of the sodium hydroxide solution was 10. The rest is the same as in example 1.
Example 3: the present embodiment is different from embodiment 1 in that: the pH of the sodium hydroxide solution was 12. The rest is the same as in example 1.
FIG. 2 is an XRD pattern, wherein A shows the XRD pattern of the aluminum hydroxide surface-modified expandable graphite flame retardant obtained in example 1, and B shows the XRD pattern of the aluminum hydroxide surface-modified expandable graphite flame retardant obtained in example 2; c represents the XRD pattern of the aluminum hydroxide surface-modified expandable graphite flame retardant obtained in example 3; d represents the XRD pattern of expandable graphite; as can be seen from FIG. 2, Al (OH) is present in the diffraction peaks of the graphite phase (PDF cards 41-1487)3Diffraction peaks of the phase (PDF card 76-1782) indicate that the aluminum hydroxide phase exists in all samples, and the successful preparation of the flame retardant is proved.
Example 4: the method for preparing the flame-retardant polyurethane foam plastic by using the aluminum hydroxide surface modified expandable graphite flame retardant is specifically completed according to the following steps:
firstly, weighing: weighing 100 parts of polyether polyol, 1 part of deionized water, 10 parts of n-pentane, 0.6 part of triethanolamine, 0.4 part of dibutyltin dilaurate, 8 parts of silicone oil, 15 parts of aluminum hydroxide surface-modified expandable graphite flame retardant, 5 parts of dioctyl adipate and 150 parts of isocyanate in parts by weight;
secondly, mixing: stirring and mixing 100 parts of polyether polyol, 1 part of deionized water, 10 parts of n-pentane, 0.6 part of triethanolamine, 0.4 part of dibutyltin dilaurate, 8 parts of silicone oil, 15 parts of aluminum hydroxide surface-modified expandable graphite flame retardant and 5 parts of dioctyl adipate weighed in the first step for 5min by using a mechanical stirrer to obtain a mixture;
thirdly, curing: and (3) adding the weighed 150 parts of isocyanate in the step (I) into the mixture obtained in the step (II), stirring for 10s, pouring into a mold, standing until the foaming is complete, transferring into an oven, and curing for 2h at the temperature of 70 ℃ to obtain the flame-retardant polyurethane foam plastic.
Example 5: the present embodiment is different from embodiment 4 in that: in the first step, 100 parts of polyether polyol, 1 part of deionized water, 10 parts of n-pentane, 0.6 part of triethanolamine, 0.4 part of dibutyltin dilaurate, 8 parts of silicone oil, 15 parts of aluminum hydroxide surface-modified expandable graphite flame retardant, 10 parts of dioctyl adipate and 150 parts of isocyanate are weighed according to parts by weight. The rest is the same as in example 4.
Example 6: the present embodiment is different from embodiment 4 in that: in the first step, 100 parts of polyether polyol, 1 part of deionized water, 10 parts of n-pentane, 0.6 part of triethanolamine, 0.4 part of dibutyltin dilaurate, 8 parts of silicone oil, 15 parts of aluminum hydroxide surface-modified expandable graphite flame retardant, 15 parts of dioctyl adipate and 150 parts of isocyanate are weighed according to parts by weight. The rest is the same as in example 4.
Example 7: adipic acid dioctyl-free comparative example:
firstly, weighing: weighing 100 parts of polyether polyol, 1 part of deionized water, 10 parts of n-pentane, 0.6 part of triethanolamine, 0.4 part of dibutyltin dilaurate, 8 parts of silicone oil, 15 parts of aluminum hydroxide surface-modified expandable graphite flame retardant and 150 parts of isocyanate according to parts by weight;
secondly, mixing: stirring and mixing 100 parts of polyether polyol, 1 part of deionized water, 10 parts of n-pentane, 0.6 part of triethanolamine, 0.4 part of dibutyltin dilaurate, 8 parts of silicone oil and 15 parts of aluminum hydroxide surface-modified expandable graphite flame retardant by using a mechanical stirrer for 5min to obtain a mixture;
thirdly, curing: and (3) adding the weighed 150 parts of isocyanate in the step (I) into the mixture obtained in the step (II), stirring for 10s, pouring into a mold, standing until the foaming is complete, transferring into an oven, and curing for 2h at the temperature of 70 ℃ to obtain the flame-retardant polyurethane foam plastic.
Example 8: the present embodiment is different from embodiment 7 in that: in the first step, 100 parts of polyether polyol, 1 part of deionized water, 10 parts of n-pentane, 0.6 part of triethanolamine, 0.4 part of dibutyltin dilaurate, 8 parts of silicone oil, 5 parts of aluminum hydroxide surface-modified expandable graphite flame retardant and 150 parts of isocyanate are weighed according to parts by weight. The rest is the same as in example 7.
Example 9: the present embodiment is different from embodiment 7 in that: in the first step, 100 parts of polyether polyol, 1 part of deionized water, 10 parts of n-pentane, 0.6 part of triethanolamine, 0.4 part of dibutyltin dilaurate, 8 parts of silicone oil, 10 parts of aluminum hydroxide surface-modified expandable graphite flame retardant and 150 parts of isocyanate are weighed according to parts by weight. The rest is the same as in example 7.
Example 10: the present embodiment is different from embodiment 7 in that: in the first step, 100 parts of polyether polyol, 1 part of deionized water, 10 parts of n-pentane, 0.6 part of triethanolamine, 0.4 part of dibutyltin dilaurate, 8 parts of silicone oil, 20 parts of aluminum hydroxide surface-modified expandable graphite flame retardant and 150 parts of isocyanate are weighed according to parts by weight. The rest is the same as in example 7.
Preparing the expandable graphite and the flame-retardant polyurethane foam plastics obtained in the embodiments 4 to 10 into a strip-shaped test piece to be tested, wherein the length, the width and the thickness of the strip-shaped test piece to be tested are 130mm, 6.5mm and 3mm, and then determining the limiting oxygen index LOI of the strip-shaped test piece to be tested according to GB/T2406-2009; measuring the heat conductivity coefficient of the strip-shaped piece to be tested according to GB/T3399-1982; measuring the compression strength of the strip-shaped piece to be tested according to GB/T8813-1988; the test results are shown in table 1.
TABLE 1
From table 1, it can be seen from comparison of expandable graphite with the flame-retardant polyurethane foams obtained in examples 7 to 10 that the flame retardant prepared by hydrothermal method using aluminum hydroxide to prepare the aluminum hydroxide surface-modified expandable graphite flame retardant can significantly improve the flame retardant property of expandable graphite, and the limiting oxygen index LOI of the expandable graphite reaches over 27%; and the comparison among the flame-retardant polyurethane foams obtained in examples 7 to 10 shows that the flame-retardant polyurethane foams used under different conditions can be prepared by changing the addition amount of the aluminum hydroxide surface-modified expandable graphite flame retardant.
As can be seen from the comparison between the flame-retardant polyurethane foams obtained in examples 4 to 6 and the flame-retardant polyurethane foams obtained in examples 7 to 10, the flame-retardant polyurethane foam obtained by adding dioctyl adipate to the raw materials still has good flame-retardant property, the compression strength of expandable graphite can be remarkably improved, and the compression strength of the flame-retardant polyurethane foam obtained in example 4 reaches 0.162 MPa.
Claims (10)
1. The preparation method of the aluminum hydroxide surface modified expandable graphite flame retardant is characterized by comprising the following steps: the expandable graphite flame retardant with the modified aluminum hydroxide surface is prepared by taking sodium hydroxide, aluminum hydroxide and expandable graphite as raw materials and adopting a hydrothermal method.
2. The method of claim 1, wherein the aluminum hydroxide surface-modified expandable graphite flame retardant comprises 30-45 wt% of aluminum hydroxide.
3. The method for preparing the aluminum hydroxide surface-modified expandable graphite flame retardant according to claim 1, wherein the hydrothermal method comprises the following specific operation processes: placing expandable graphite and aluminum hydroxide into a reaction kettle, adding a sodium hydroxide solution with the pH value of 10-12, uniformly stirring, covering the reaction kettle, heating to 200-220 ℃, reacting at the temperature of 200-220 ℃ for 1.5-2.5 h, cooling to room temperature to obtain a solid-liquid mixture, and sequentially filtering, washing and vacuum drying to obtain the aluminum hydroxide surface modified expandable graphite flame retardant.
4. The preparation method of the aluminum hydroxide surface modified expandable graphite flame retardant according to claim 3, wherein the mass ratio of the expandable graphite to the aluminum hydroxide is 1 (1-1.2); the volume ratio of the mass of the expandable graphite to the sodium hydroxide solution with the pH value of 11 is 1g (9-12) mL.
5. The method for preparing the aluminum hydroxide surface-modified expandable graphite flame retardant according to claim 4, wherein the filtering is performed by the following steps: and filtering the solid-liquid mixture by using filter paper to obtain a filter cake.
6. The method for preparing the aluminum hydroxide surface-modified expandable graphite flame retardant according to claim 5, characterized in that the washing operation is as follows: and washing the filter cake with deionized water for 3-5 times to obtain a washed solid, wherein the volume ratio of the mass of the filter cake to the volume of the deionized water in a single washing is 1g (30-50) mL.
7. The method for preparing the aluminum hydroxide surface-modified expandable graphite flame retardant according to claim 6, wherein the vacuum drying is specifically performed as follows: and (3) putting the washed solid in a vacuum drying oven, and carrying out vacuum drying for 4-6 h at the temperature of 60-80 ℃ to obtain the aluminum hydroxide surface modified expandable graphite flame retardant.
8. The method for preparing flame retardant polyurethane foam by using the aluminum hydroxide surface modified expandable graphite flame retardant of claim 1, which is characterized by comprising the following steps:
firstly, weighing: weighing 100 parts of polyether polyol, 0.8-1.2 parts of deionized water, 8-12 parts of n-pentane, 0.4-0.8 part of triethanolamine, 0.3-0.5 part of dibutyltin dilaurate, 6-10 parts of silicone oil, 5-20 parts of aluminum hydroxide surface modified expandable graphite flame retardant, 5-15 parts of dioctyl adipate and 130-170 parts of isocyanate according to parts by weight;
secondly, mixing: stirring and mixing 100 parts of polyether polyol, 0.8-1.2 parts of deionized water, 8-12 parts of n-pentane, 0.4-0.8 part of triethanolamine, 0.3-0.5 part of dibutyltin dilaurate, 6-10 parts of silicone oil, 5-20 parts of aluminum hydroxide surface modified expandable graphite flame retardant and 5-15 parts of dioctyl adipate weighed in the first step to obtain a mixture;
thirdly, curing: and (3) adding 130-170 parts of isocyanate weighed in the step (I) into the mixture obtained in the step (II), firstly stirring for 7-13 s, then pouring into a mold, standing until the foaming is complete, then transferring into an oven, and curing for 1.7-2.3 h at the temperature of 60-80 ℃ to obtain the flame-retardant polyurethane foam plastic.
9. The method for preparing the aluminum hydroxide surface modified expandable graphite flame retardant according to claim 8, wherein in the first step, 100 parts of polyether polyol, 1 part of deionized water, 10 parts of n-pentane, 0.6 part of triethanolamine, 0.4 part of dibutyltin dilaurate, 8 parts of silicone oil, 5-20 parts of the aluminum hydroxide surface modified expandable graphite flame retardant, 5-15 parts of dioctyl adipate and 150 parts of isocyanate are weighed according to the parts by weight.
10. The method for preparing the aluminum hydroxide surface-modified expandable graphite flame retardant according to claim 9, wherein the stirring and mixing in the second step are specifically performed as follows: stirring and mixing for 4-10 min by a mechanical stirrer.
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|---|---|---|---|---|
| CN107345002A (en) * | 2016-05-06 | 2017-11-14 | 武汉理工大学 | A kind of expansible graphite fire retardant of hydroxide β-cyclodextrin and preparation method thereof |
| CN107641221A (en) * | 2016-07-22 | 2018-01-30 | 武汉理工大学 | A kind of hydroxide-modified expansible graphite fire retardant and preparation method thereof |
| US20200362133A1 (en) * | 2019-05-17 | 2020-11-19 | L & P Property Management Company | Expandable Graphite Flame Retardant Coating for Polyurethane and Latex Foam |
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| CN107345002A (en) * | 2016-05-06 | 2017-11-14 | 武汉理工大学 | A kind of expansible graphite fire retardant of hydroxide β-cyclodextrin and preparation method thereof |
| CN107641221A (en) * | 2016-07-22 | 2018-01-30 | 武汉理工大学 | A kind of hydroxide-modified expansible graphite fire retardant and preparation method thereof |
| US20200362133A1 (en) * | 2019-05-17 | 2020-11-19 | L & P Property Management Company | Expandable Graphite Flame Retardant Coating for Polyurethane and Latex Foam |
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