CN113817225B - Composite warm-mixing flame-retardant modifier, preparation method thereof, modified capsule and application thereof - Google Patents

Composite warm-mixing flame-retardant modifier, preparation method thereof, modified capsule and application thereof Download PDF

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CN113817225B
CN113817225B CN202111117300.4A CN202111117300A CN113817225B CN 113817225 B CN113817225 B CN 113817225B CN 202111117300 A CN202111117300 A CN 202111117300A CN 113817225 B CN113817225 B CN 113817225B
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flame retardant
mixing
warm
flame
retardant
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CN113817225A (en
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陈辉强
姚建国
鲜江林
廖伟
马俊
李雁翔
唐戈
王雄
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Guang'an Transportation Investment Construction Development Group Co ltd
Chongqing Jiaotong University
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Guang'an Transportation Investment Construction Development Group Co ltd
Chongqing Jiaotong University
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Abstract

The invention belongs to the technical field of warm-mixing and flame-retardant materials, and discloses a composite warm-mixing flame-retardant modifier, a preparation method thereof, a modified capsule and application thereof. The modified capsule is prepared by uniformly mixing a warm-mixing agent, a flame retardant subjected to surface modification by a coupling agent, a synergist and a smoke suppressant, adding a binder, heating, cooling and granulating to obtain modifier particles, and encapsulating the modifier particles in a low-density polyethylene capsule shell. The modified capsule is used in the production process of the asphalt mixture paved on the long and large tunnel, and can realize the dual purposes of low smoke during the construction of the asphalt mixture of the extra-long tunnel and safety during operation only by directly putting the capsule in a mixing pot of the asphalt mixture, thereby greatly simplifying the production process of the warm-mixed flame-retardant asphalt mixture, improving the production efficiency, saving the cost, and obviously improving the production efficiency with simple and convenient operation.

Description

Composite warm-mixing flame-retardant modifier, preparation method thereof, modified capsule and application thereof
Technical Field
The invention belongs to the technical field of warm-mixing and flame-retardant materials, and particularly relates to a composite warm-mixing flame-retardant modifier, a preparation method thereof, a modified capsule and application thereof.
Background
In recent years, with the rapid development of highways in China, particularly mountain areas, the large and large tunnels of the highways in the mountain areas occupy a large proportion. Asphalt pavement is widely applied to pavement of long and large tunnels of expressways due to a plurality of technical advantages compared with cement concrete pavement.
At present, the tunnel pavement tends to be more and more the warm mix flame retardant asphalt concrete with low asphalt smoke release amount, reliable construction quality and high later-stage operation safety coefficient. However, the technical bottleneck faced by the good warm-mix flame-retardant concrete is limited to a certain extent by the low production efficiency caused by the various additives and the complicated mixing process, in addition to the technical difficulty of warm-mix flame retardance.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a composite warm-mixing flame retardant modifier, a preparation method thereof, a modified capsule and application thereof.
The technical scheme adopted by the invention is as follows: the composite warm mixing flame retardant modifier is mainly prepared from the following raw materials in parts by mass:
80-100 parts of flame retardant, 3-8 parts of warm mixing agent, 30-70 parts of synergist and 20-50 parts of smoke suppressant;
the warm mixing agent is artificial zeolite powder;
the water content of the warm mixing agent is about 21wt%, and the specific surface area is 355-1000m 2 /g。
Preferably, the flame retardant is an inorganic flame retardant;
the flame retardant comprises a mixture of magnesium hydroxide and aluminum hydroxide;
the mass ratio of the magnesium hydroxide to the aluminum hydroxide is 3-5;
the synergist is an inorganic phosphorus synergist;
the inorganic phosphorus synergist comprises ammonium polyphosphate;
the smoke suppressant is red phosphorus.
The flame retardant is prepared by adopting a mode of a mixture of magnesium hydroxide and aluminum hydroxide, and aims to aim at two stages of construction and operation. Due to the difference of corresponding flame retardant mechanisms, the decomposition temperature of the aluminum hydroxide is relatively low, and the aluminum hydroxide is mainly decomposed in the mixing and construction processes of the mixture, so that the flame retardant and smoke suppression effects are achieved. The magnesium hydroxide has higher decomposition temperature and is mainly used for decomposing under the condition of fire disaster in the operation process of the tunnel, thereby playing a role of flame retardance. The two raw materials have low cost and belong to environment-friendly raw materials.
The synergist is an inorganic phosphorus synergist, and refers to a synergist containing phosphorus elements, namely a phosphorus synergist, and comprises organic and inorganic synergists.
Ammonium polyphosphate of formula (NH) 4 ) n+2 P n O 3n+1 Wherein n is 80-100. It is a high-efficiency environment-friendly synergist with no toxicity, no odor, low hygroscopicity and high thermal stability.
Preferably, the particle size of the flame retardant is 500-1000 meshes;
the particle size of the smoke suppressant is 5-20 mu m, and the density is 2.10-2.30 g/cm 3 。
Preferably, the red phosphorus is P 4 The single bonds of the tetrahedra form highly polymeric structures of chains or rings.
The red phosphorus is P 4 The tetrahedral single bond forms a chain or ring high polymer structure, and because the same substance has different structures although the chemical composition is the same, the presented chemical properties are different, and the red phosphorus smoke suppression effect of the structure is the best.
Preferably, the flame retardant is a mixture of inorganic flame retardants of magnesium hydroxide and aluminum hydroxide surface-modified by coupling agent titanate;
the surface modification method comprises the following steps:
a. firstly, putting magnesium hydroxide and aluminum hydroxide into a mixing pot with a stirring device in proportion, starting stirring, controlling the rotating speed at 100-300 r/min, and stirring for 3-6 min;
b. absolute ethyl alcohol and titanate coupling agent are used according to the volume ratio of 1:100, diluting;
c. uniformly spraying the solution obtained in the step b onto the flame retardant in the mixing pot, and uniformly mixing;
d. and d, standing the product obtained in the step c in an oven at the temperature of 100-120 ℃ for 1.5-2 h, drying, and cooling to normal temperature to obtain the surface modified flame retardant.
The mass ratio of the flame retardant is 1/4-3/4, and the particle size range of the flame retardant is 500-1000 meshes.
The titanate coupling agent is a titanate coupling agent CS201.
A preparation method of a composite warm-mixing flame retardant modifier comprises the following steps:
A. selecting a synergist, a smoke suppressant, a warm mixing agent and a flame retardant according to corresponding proportions, uniformly mixing, adding an adhesive through a stirring device at the rotating speed of 60-150 r/min, heating to 115-125 ℃, and uniformly mixing again after the adhesive is melted;
B. adjusting the rotating speed of the stirring device to 200-300 r/min, continuously stirring for 2-5 min, stopping stirring, cooling to room temperature, and granulating to obtain a finished product with the particle size of 20-60 meshes.
Preferably, the binder is natural rosin.
The natural rosin has a melting point of 110-135 ℃ and a chemical formula of C 20 H 30 O 2 The density is 1.060-1.085 g/cm 3 。
The preparation method is characterized in that the adhesive is added, and the superfine powder (synergist, smoke suppressant and flame retardant) and the warm mixing agent are bonded together, so that the subsequent granulation process is facilitated.
Preferably, the mass ratio of the total mass of the synergist, the smoke suppressant, the warm-mix agent and the flame retardant to the adhesive is 50-100:10-35.
A composite warm-mixing flame-retardant modified capsule, which is obtained by filling a capsule shell with the composite warm-mixing flame-retardant modifier obtained by the preparation method of any one of claims 6 to 8;
the capsule shell is made of polyethylene;
the diameter of the cross section of the capsule shell is 3-10 mm, and the length is 30-60 mm.
The capsule shell is made of pure low-density polyethylene material. The capsule shell is melted when being heated, and can play a role in modifying the performance of the asphalt.
The constituent materials in the composite warm-mixing flame-retardant modified capsule can not generate chemical action with each other, and can fully play a good synergistic flame-retardant role. The working mechanism of the composite warm mixing flame-retardant modified capsule is briefly described as follows: in the process of mixing and paving the asphalt mixture, the capsule shell can be directly used as an asphalt modifier to be mixed and dissolved with the asphalt, the aluminum hydroxide can dehydrate and absorb heat at 140-150 ℃, the aluminum hydroxide and the warm mixing agent synergistically act to reduce the mixing temperature, reduce the smoke release amount in the process of paving the tunnel and play a role of warm mixing; under the condition of sudden fire hazard in the tunnel operation process, the flame retardant (aluminum hydroxide and magnesium hydroxide), the synergist and the smoke suppressant can fully exert good synergistic flame retardant action and smoke suppression action, and ensure the operation safety of the highway tunnel, particularly the long and large highway tunnel.
An application of the composite warm-mixing flame-retardant modified capsule in paving a long and large tunnel asphalt pavement, wherein the composite warm-mixing flame-retardant modified capsule in claim 9 is adopted.
The above-mentioned growth means that the area of the whole asphalt pavement is large.
The invention has the beneficial effects that:
the invention provides a composite warm-mixing flame-retardant modified capsule, which is prepared by uniformly mixing a warm-mixing agent, a flame retardant subjected to surface modification by a coupling agent, a synergist, a smoke suppressant and an adhesive, heating for bonding, cooling for granulation to obtain modifier particles, and encapsulating the modifier particles in a low-density polyethylene capsule shell. The modified capsule is used in the production process of the asphalt mixture paved on the long and large tunnel, and the purpose of being suitable for paving the tunnel asphalt pavement for long time and being warm-mix flame retardant can be realized only by directly putting the capsule in a mixing pot of the asphalt mixture, and the production efficiency is remarkably improved.
The modifier mixes the flame retardant, the synergist, the smoke inhibitor and the warm-mix agent according to a certain proportion, not only fully plays roles of warm mixing and flame retardance, but also realizes double purposes of low smoke and safety in operation during construction of the asphalt mixture of the extra-long tunnel by utilizing the synergistic flame retardance of the synergist, the smoke inhibitor and the flame retardant, greatly simplifies the production process of the warm-mix flame-retardant asphalt mixture, improves the production efficiency and saves the cost.
The modifier integrates a plurality of composite flame retardants with high flame retardant efficiency and a warm mixing agent with good cooling effect in a capsule form to prepare the warm mixing flame retardant composite modified capsule, has the characteristics of warm mixing cooling and flame retardance, can be directly put into an asphalt mixture mixing pot in a capsule form, is simple to operate, and remarkably improves the production efficiency.
The invention not only meets the requirements of warm mixing and cooling in the process of mixing, transporting and paving the tunnel pavement asphalt mixture, realizes that the smoke quantity released by asphalt during the construction of the asphalt mixture in the process of tunnel pavement is greatly reduced, ensures the safety of the tunnel in the operation process, but also greatly simplifies the complicated processes and flows brought by various additives, thereby obviously improving the production efficiency and achieving the purpose of reducing the construction cost.
Detailed Description
The present invention will be further explained with reference to specific examples. It will be appreciated by those skilled in the art that the following examples, which are set forth to illustrate the present invention, are intended to be part of the present invention, but not to be construed as limiting the scope of the present invention. The reagents used are conventional products which are commercially available.
Example 1:
a preparation method of a composite warm-mixing flame-retardant modified capsule comprises the following raw materials in parts by weight:
obtaining the composite warm-mixing flame-retardant modifier: 100 g of flame retardant (30 g of aluminum hydroxide and 70 g of magnesium hydroxide), 10 g of artificial zeolite powder, 65 g of ammonium polyphosphate and 25 g of red phosphorus; 80 g of natural rosin.
The flame retardant is a mixture of aluminum hydroxide (500-800 meshes) and magnesium hydroxide with the granularity (800-1000 meshes) after the surface modification by the absolute ethanol solution of the titanate coupling agent CS201.
The synergist is an unbranched long chain polymer: and (3) ammonium polyphosphate. The smoke suppressant is P 4 The tetrahedral single bonds form a powder of highly polymeric structure of chains or rings. The capsule shell is made of low-density polyethylene.
In this embodiment, the preparation method of the flame retardant includes the following steps:
a. selecting two mixed flame retardants of magnesium hydroxide and aluminum hydroxide according to corresponding proportions, uniformly mixing, putting into an oven at 85 ℃, heating for 1h, taking out, adding an absolute ethyl alcohol solution of a titanate coupling agent CS-201, and stirring for 5min at a rotating speed of 100r/min by using a multifunctional stirrer;
b. and (b) putting the article obtained in the step a into a drying oven at 110 ℃ and heating for 1h, and taking out to obtain the flame retardant subjected to surface modification by the anhydrous ethanol solution of the titanate coupling agent CS201.
Uniformly mixing the flame retardant, the warm-mix agent, the smoke suppressant, the synergist and the adhesive in proportion, stirring by using a multifunctional stirrer at the rotating speed of 60r/min, heating until the adhesive is molten, continuously stirring at the rotating speed of 200r/min for 5min, cooling to room temperature for granulation, and controlling the particle size to be 20-30 meshes to obtain the composite warm-mix flame retardant modifier particles.
The preparation method of the composite warm-mixing flame-retardant modified capsule suitable for asphalt pavement of the long and large road tunnel comprises the following steps: the composite warm-mixing flame-retardant modified capsule required by the invention is prepared by filling the composite warm-mixing flame-retardant modifier particles into a low-density polyethylene capsule shell by adopting a full-automatic capsule filling machine, and the capsule appearance size is as follows: the cross section diameter is 3mm, and the length is 30mm.
Example 2:
a preparation method of a composite warm-mixing flame-retardant modified capsule comprises the following raw materials in parts by weight:
obtaining the composite warm-mixing flame-retardant modifier: 80 g of flame retardant (40 g of aluminum hydroxide and 40 g of magnesium hydroxide), 3 g of artificial zeolite powder, 30g of ammonium polyphosphate and 20 g of red phosphorus; 44 g of natural rosin.
The flame retardant is a mixture of aluminum hydroxide (500-800 meshes) and magnesium hydroxide with the granularity (800-1000 meshes) after the surface modification by the absolute ethanol solution of the titanate coupling agent CS201.
The synergist is an unbranched long chain polymer: and (4) ammonium polyphosphate. The smoke suppressant is P 4 The tetrahedral single bonds form a powder of highly polymeric structure of chains or rings. The capsule shell is made of low-density polyethylene.
In this embodiment, the preparation method of the flame retardant includes the following steps:
a. selecting two mixed flame retardants of magnesium hydroxide and aluminum hydroxide according to corresponding proportions, uniformly mixing, putting into a baking oven at 95 ℃, heating for 2h, taking out, adding an absolute ethyl alcohol solution of a titanate coupling agent CS-201, and stirring for 20min at a rotating speed of 300r/min by using a multifunctional stirrer;
b. and (b) heating the article obtained in the step (a) in a drying oven at 110 ℃ for 2h, and taking out the article to obtain the flame retardant subjected to surface modification by the anhydrous ethanol solution of the titanate coupling agent CS201.
Uniformly mixing the flame retardant, the warm-mix agent, the smoke suppressant, the synergist and the adhesive in proportion, stirring by using a multifunctional stirrer at the rotating speed of 150r/min, heating until the adhesive is molten, continuously stirring at the rotating speed of 300r/min for 10min, cooling to room temperature for granulation, and controlling the particle size of particles to be 50-60 meshes to obtain the composite warm-mix flame retardant modifier particles.
The preparation method of the composite warm-mixing flame-retardant modified capsule suitable for asphalt pavement of the long and large road tunnel comprises the following steps: the composite warm-mixing flame-retardant modified capsule required by the invention is prepared by filling the composite warm-mixing flame-retardant modifier particles into a low-density polyethylene capsule shell by adopting a full-automatic capsule filling machine, and the capsule appearance size is as follows: the cross section diameter is 10mm, and the length is 60mm.
Example 3:
obtaining the composite warm-mixing flame-retardant modifier: 100 g of flame retardant (40 g of aluminum hydroxide and 60 g of magnesium hydroxide), 8 g of artificial zeolite powder, 70 g of ammonium polyphosphate and 50 g of red phosphorus; 46 g of natural rosin.
Example 4:
obtaining the composite warm mixing flame retardant modifier: 100 g of flame retardant (wherein 50 g of aluminum hydroxide and 50 g of magnesium hydroxide), 13 g of artificial zeolite powder, 55 g of ammonium polyphosphate and 32 g of red phosphorus; and 70 g of natural rosin.
Example 5:
obtaining the composite warm-mixing flame-retardant modifier: 100 g of flame retardant (wherein 50 g of aluminum hydroxide and 50 g of magnesium hydroxide), 16 g of artificial zeolite powder, 45 g of ammonium polyphosphate and 39 g of red phosphorus; 70 g of natural rosin.
Example 6:
obtaining the composite warm-mixing flame-retardant modifier: 100 g of flame retardant (wherein 50 g of aluminum hydroxide and 50 g of magnesium hydroxide), 19 g of artificial zeolite powder, 40 g of ammonium polyphosphate and 41 g of red phosphorus; 70 g of natural rosin.
Example 7:
obtaining the composite warm mixing flame retardant modifier: 100 g of flame retardant (wherein 50 g of aluminum hydroxide and 50 g of magnesium hydroxide), 8 g of artificial zeolite powder, 70 g of ammonium polyphosphate and 50 g of red phosphorus; 45.6 g of natural rosin.
Experimental example:
the preparation method and treatment protocol described above in example 1 were used.
The flame retardant modifier of example 1/4/5/6 is added into SBS flame retardant modified asphalt at 145 ℃ after being prepared according to the parts by weight, the temperature is kept at 145 +/-5 ℃, four warm mixing flame retardant modifiers are prepared after being sheared for 0.5h by a high speed shearing machine under the condition of 5500r/min, and the flame retardant performance and the road performance are listed in Table 1.
TABLE 1 70 # Pavement performance and flame retardant performance of matrix asphalt and several kinds of warm-mixed flame-retardant low-smoke type modified asphalt
Figure BDA0003275940000000081
Figure BDA0003275940000000091
The same-grade aggregate, SBS modified asphalt and the composite warm-mixed flame-retardant modified capsules prepared by the 4 examples are directly put into a mixing pot of asphalt mixture in sequence for mixing to obtain 4 kinds of warm-mixed flame-retardant asphalt mixtures AC-13C, the road performance of the warm-mixed flame-retardant asphalt mixtures is tested respectively, and the test results are compared with that of SBS modified asphalt mixtures and are listed in Table 2.
TABLE 2 road Properties of several AC-13 asphalt mixtures
Figure BDA0003275940000000092
And (4) conclusion: the experimental results of the comparative example and the SBS modified asphalt and the mixture thereof show that the addition of the warm-mixed flame-retardant capsule has obvious influence on the pavement performance and the combustion characteristic of the SBS modified asphalt and the mixture thereof.
Specifically, compared with SBS modified asphalt, the modified asphalt provided by the embodiment has a relatively obvious cooling effect, the cooling amplitude is increased along with the increase of the mixing amount of the warm-mix agent, the penetration degree and the ductility are reduced, the softening point is increased, the smoke density is reduced remarkably, the amplitude is in linear negative correlation with the mixing amount of the smoke inhibitor, the oxygen index is increased remarkably, and the oxygen index is in linear positive correlation with the mixing amount of the flame retardant and the smoke inhibitor, so that the warm-mix flame-retardant asphalt has excellent road performance, and also has good flame retardance and low smoke. Compared with the SBS modified asphalt AC13 mixture, the dynamic stability and the freeze-thaw cleavage strength of the mixture are both increased slightly, and the maximum bending tensile strain is slightly reduced, which shows that the warm-mixed flame-retardant capsule improves the high-temperature performance and the water damage resistance of the mixture, and causes the small reduction of the low-temperature performance. Considering the environmental characteristics of 'warm in winter and cool in summer' of the long and large tunnel, the small reduction of the low-temperature performance does not cause the use durability of the tunnel asphalt surface layer; on the contrary, the better water damage resistance of the warm-mix flame-retardant asphalt mixture can improve the service durability of the warm-mix flame-retardant asphalt mixture.
The present invention is not limited to the above alternative embodiments, and any other various products can be obtained by anyone in the light of the present invention, and all fall within the protection scope of the present invention. The above-described embodiments should not be construed as limiting the scope of the present invention, and it will be understood by those skilled in the art that modifications may be made to the embodiments described in the foregoing embodiments, or that equivalents may be substituted for part or all of the features thereof, without departing from the scope of the present invention, and that such modifications or substitutions do not depart from the essence of the corresponding embodiments.

Claims (9)

1. The composite warm mixing flame retardant modifier is characterized by being prepared from the following raw materials in parts by mass:
80-100 parts of flame retardant, 3-8 parts of warm mixing agent, 30-70 parts of synergist and 20-50 parts of smoke suppressant;
the warm mixing agent is artificial zeolite powder;
the water content of the warm mixing agent is 21wt%, and the specific surface area is 355-1000m 2 /g；
The flame retardant comprises a mixture of magnesium hydroxide and aluminum hydroxide;
the mass ratio of the magnesium hydroxide to the aluminum hydroxide is 3-5;
the smoke suppressant is red phosphorus; the red phosphorus is P 4 The single bonds of the tetrahedra form highly polymeric structures of chains or rings.
2. The composite warm-mix flame retardant modifier according to claim 1, wherein the flame retardant is an inorganic flame retardant; the synergist is an inorganic phosphorus synergist;
the inorganic phosphorus synergist comprises ammonium polyphosphate.
3. The composite warm-mix flame retardant modifier of claim 2, wherein the particle size of the flame retardant is 500-1000 meshes;
the particle size of the smoke suppressant is 5-20 mu m, and the density is 2.10-2.30 g/cm 3 。
4. The composite warm-mix flame retardant modifier of claim 2, wherein the flame retardant is a mixture of inorganic flame retardants of magnesium hydroxide and aluminum hydroxide surface-modified by coupling agent titanate;
the surface modification method comprises the following steps:
a. firstly, putting magnesium hydroxide and aluminum hydroxide into a mixing pot with a stirring device in proportion, starting stirring, controlling the rotating speed at 100-300 r/min, and stirring for 3-6 min;
b. absolute ethyl alcohol and titanate coupling agent are used according to the volume ratio of 1:100, diluting;
c. c, uniformly spraying the solution obtained in the step b onto the flame retardant in the mixing pot, and uniformly mixing;
d. and d, standing the product obtained in the step c in an oven at the temperature of 100-120 ℃ for 1.5-2 h, drying, and cooling to normal temperature to obtain the surface modified flame retardant.
5. A method for preparing the composite warm-mix flame retardant modifier according to any one of claims 1 to 4, wherein the method comprises the following steps:
A. selecting a synergist, a smoke suppressant, a warm mixing agent and a flame retardant according to corresponding proportions, uniformly mixing, adding an adhesive through a stirring device at the rotating speed of 60-150 r/min, heating to 115-125 ℃, and uniformly mixing again after the adhesive is melted;
B. adjusting the rotating speed of the stirring device to 200-300 r/min, continuing stirring for 2-5 min, stopping stirring, cooling to room temperature, and obtaining the finished product with the granulation particle size of 20-60 meshes.
6. The preparation method of the composite warm-mixed flame retardant modifier as claimed in claim 5, wherein the adhesive is natural rosin.
7. The preparation method of the composite warm mix flame retardant modifier according to claim 5, wherein the mass ratio of the total mass of the synergist, the smoke suppressant, the warm mix agent and the flame retardant to the adhesive is 50-100:10-35.
8. A composite warm mixing flame retardant modified capsule is characterized in that the modified capsule is obtained by filling the composite warm mixing flame retardant modifier obtained by the preparation method of any one of the claims 5 to 7 into a capsule shell;
the capsule shell is made of polyethylene;
the diameter of the cross section of the capsule shell is 3-10 mm, and the length is 30-60 mm.
9. The application of the composite warm-mixing flame-retardant modified capsule is characterized in that the composite warm-mixing flame-retardant modified capsule in claim 8 is applied to paving of asphalt pavements of long and large tunnels.
CN202111117300.4A 2021-09-23 2021-09-23 Composite warm-mixing flame-retardant modifier, preparation method thereof, modified capsule and application thereof Active CN113817225B (en)

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