CN114381108A - Flame-retardant composite anchor rod and preparation method thereof - Google Patents
Flame-retardant composite anchor rod and preparation method thereof Download PDFInfo
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- CN114381108A CN114381108A CN202210143411.0A CN202210143411A CN114381108A CN 114381108 A CN114381108 A CN 114381108A CN 202210143411 A CN202210143411 A CN 202210143411A CN 114381108 A CN114381108 A CN 114381108A
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 78
- 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 77
- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims description 19
- 239000000463 material Substances 0.000 claims abstract description 51
- 239000000835 fiber Substances 0.000 claims abstract description 46
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 31
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 29
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 26
- 150000002367 halogens Chemical class 0.000 claims abstract description 26
- 229920006337 unsaturated polyester resin Polymers 0.000 claims abstract description 26
- 229920000728 polyester Polymers 0.000 claims abstract description 24
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 20
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 20
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 20
- 239000010941 cobalt Substances 0.000 claims abstract description 20
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 20
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 230000002787 reinforcement Effects 0.000 claims abstract description 10
- 229920005989 resin Polymers 0.000 claims description 33
- 239000011347 resin Substances 0.000 claims description 33
- 238000004804 winding Methods 0.000 claims description 32
- 238000003756 stirring Methods 0.000 claims description 19
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- 229920002748 Basalt fiber Polymers 0.000 claims description 12
- 238000007598 dipping method Methods 0.000 claims description 10
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 9
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 9
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000005470 impregnation Methods 0.000 claims description 8
- NOBYOEQUFMGXBP-UHFFFAOYSA-N (4-tert-butylcyclohexyl) (4-tert-butylcyclohexyl)oxycarbonyloxy carbonate Chemical compound C1CC(C(C)(C)C)CCC1OC(=O)OOC(=O)OC1CCC(C(C)(C)C)CC1 NOBYOEQUFMGXBP-UHFFFAOYSA-N 0.000 claims description 7
- BZQKBFHEWDPQHD-UHFFFAOYSA-N 1,2,3,4,5-pentabromo-6-[2-(2,3,4,5,6-pentabromophenyl)ethyl]benzene Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1CCC1=C(Br)C(Br)=C(Br)C(Br)=C1Br BZQKBFHEWDPQHD-UHFFFAOYSA-N 0.000 claims description 7
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 claims description 7
- OEOIWYCWCDBOPA-UHFFFAOYSA-N 6-methyl-heptanoic acid Chemical compound CC(C)CCCCC(O)=O OEOIWYCWCDBOPA-UHFFFAOYSA-N 0.000 claims description 6
- 239000003365 glass fiber Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000009775 high-speed stirring Methods 0.000 claims description 5
- 239000003292 glue Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000003245 coal Substances 0.000 abstract description 17
- 238000010276 construction Methods 0.000 abstract description 9
- 230000003993 interaction Effects 0.000 abstract description 3
- 238000005520 cutting process Methods 0.000 description 12
- 238000009966 trimming Methods 0.000 description 11
- 239000011159 matrix material Substances 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 238000005065 mining Methods 0.000 description 4
- 239000012779 reinforcing material Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 229940057404 di-(4-tert-butylcyclohexyl)peroxydicarbonate Drugs 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- QEQBMZQFDDDTPN-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy benzenecarboperoxoate Chemical compound CC(C)(C)OOOC(=O)C1=CC=CC=C1 QEQBMZQFDDDTPN-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 229920006231 aramid fiber Polymers 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229920006253 high performance fiber Polymers 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/06—Unsaturated polyesters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The invention provides a flame-retardant composite anchor rod which is prepared from the following raw materials: 150-152 parts by weight of a fiber reinforcement material; 1000 parts by weight of unsaturated polyester resin; 5-9 parts of curing agent; 2-6 parts of styrene; 10 to 24 parts by weight of calcined kaolin; 0.5 to 1.5 parts by weight of cobalt iso-octoate; 80-300 parts by weight of halogen flame retardant; 5-6 parts of polyester filament yarn. Compared with the prior art, the flame-retardant composite anchor rod provided by the invention is prepared from raw materials with specific content of components, so that the overall better interaction is realized, the product has excellent flame-retardant property on the basis of stable performance of various kinds, the safety of the anchor rod in the construction process is improved, and the flame-retardant composite anchor rod can be used in the fields with higher requirements on construction environment, such as coal mine tunnels and the like.
Description
Technical Field
The invention relates to the technical field of anchor rods, in particular to a flame-retardant composite anchor rod and a preparation method thereof.
Background
In the field of coal mines, in order to keep the stability of a coal mine tunnel and prevent surrounding rocks from caving or deforming too much, supporting is generally required after the tunnel is tunneled. At present, support products such as anchor rods, anchor cables, anchor nets and the like used in the field of support of coal mine roadways in China are mature and are applied to various developed coal mines in China. The anchor rod is used as a necessary means for the current support, and has the function of stable support in coal seams with different properties and different geologies. The most used anchor rods on the common coal mining surface are composite material glass fiber reinforced plastic anchor rods which have the advantages of light weight, high strength, excellent acid and alkali resistance and long service life. Considering the safety factor, the composite anchor rod like the coal mining side should have flame retardant performance.
In the published data, the top of a coal mine tunnel is generally supported by a metal anchor rod, two side walls of the coal mine tunnel are generally supported by common composite anchor rods and anchor nets, and a layer of concrete is finally paved on the outer layer of the support for reinforcement. The metal anchor rod is a rod-shaped metal rod body formed by round steel after being fixed and cut off and pressed by a machine and then being subjected to a thread rolling process, the torque and the shear strength are high, if the metal anchor rod is used on a coal mining side, cutting cannot be performed after recovery, and the metal anchor rod needs to be taken out of an anchor hole one by one, so that the construction time is prolonged; and the flame retardant property is poor or no, so that sparks can be generated under the condition of high requirement on the coal mine environment, and the safety of a mine hole is influenced. The common composite material anchor rod is a rod-shaped product which is prepared by taking epoxy resin (unsaturated polyester resin, vinyl resin and the like) as a base material and glass fiber (basalt fiber and the like) as a reinforcing material through a pultrusion process, and also has no flame retardant property.
Disclosure of Invention
In view of the above, the invention aims to provide a flame-retardant composite anchor rod and a preparation method thereof.
The invention provides a flame-retardant composite anchor rod which is prepared from the following raw materials:
150-152 parts by weight of a fiber reinforcement material;
1000 parts by weight of unsaturated polyester resin;
5-9 parts of curing agent;
2-6 parts of styrene;
10 to 24 parts by weight of calcined kaolin;
0.5 to 1.5 parts by weight of cobalt iso-octoate;
80-300 parts by weight of halogen flame retardant;
5-6 parts of polyester filament yarn.
Preferably, the fibrous reinforcing material is selected from basalt fibers and/or glass fibers; the fiber diameter of the fiber reinforced material is 10-20 μm, the tensile strength is more than or equal to 0.1N/tex, the water content is less than or equal to 0.5%, and the content of combustible is 0.1-1%.
Preferably, the solid content of the unsaturated polyester resin is 60-75%, the viscosity of the resin is 300-1000 mPa.S, and the acid value is 10-30 mg KOH/g.
Preferably, the curing agent is prepared from the following components in percentage by mass (2-4): (1-3): 2 tert-butyl peroxybenzoate, benzoyl peroxide and bis (4-tert-butylcyclohexyl) peroxydicarbonate).
Preferably, the halogen flame retardant is prepared from the following components in percentage by mass (50-52): (30-32) decabromodiphenylethane and antimony trioxide,
or, the halogen flame retardant SZ 182.
The invention also provides a preparation method of the flame-retardant composite material anchor rod, which comprises the following steps:
a) mixing unsaturated polyester resin, a curing agent, styrene, calcined kaolin, cobalt isooctanoate and a halogen flame retardant to obtain a resin mixed material;
b) and b) dipping the fiber reinforced material by adopting the resin mixed material obtained in the step a), winding polyester filament yarns, and curing and forming to obtain the flame-retardant composite anchor rod.
Preferably, the mixing process in step a) is specifically:
uniformly mixing a curing agent and styrene to obtain a curing agent mixture; then under the condition of low-speed stirring adding the above-mentioned solidifying agent mixture into unsaturated polyester resin; then sequentially adding calcined kaolin, cobalt iso-octoate and halogen flame retardant, and stirring at a high speed to obtain a resin mixed material; the rotating speed of the low-speed stirring is 100 r/min-200 r/min; the high-speed stirring speed is 500 r/min-600 r/min, the temperature is 10-35 ℃, and the time is 10-25 min.
Preferably, the gum dipping process in the step b) specifically comprises the following steps:
pouring the resin mixed material into a glue tank, and uniformly dipping the fiber reinforced material which is arranged orderly into the resin mixed material; in the whole impregnation process, the fiber reinforced material is kept to be arranged neatly; the rubber content of the anchor rod is controlled by the tightening of the rubber extruding roller of the rubber groove, so that the rubber content is controlled to be 15-25%.
Preferably, the process of winding the polyester filament yarn in the step b) specifically comprises:
winding the impregnated fiber reinforced material in a winding area, winding the polyester filament yarn on the fiber reinforced material through a winding device, controlling the tension to be 2 Hz-2.5 Hz, and ensuring the uniform thread pitch.
Preferably, the curing process in the step b) is carried out by heating in an oven, wherein the oven has 7 temperature zones, and the heating time is 5-6 min at 340-360 ℃, 290-310 ℃, 240-260 ℃, 230-250 ℃, 220-240 ℃, 190-210 ℃ in sequence.
The invention provides a flame-retardant composite anchor rod which is prepared from the following raw materials: 150-152 parts by weight of a fiber reinforcement material; 1000 parts by weight of unsaturated polyester resin; 5-9 parts of curing agent; 2-6 parts of styrene; 10 to 24 parts by weight of calcined kaolin; 0.5 to 1.5 parts by weight of cobalt iso-octoate; 80-300 parts by weight of halogen flame retardant; 5-6 parts of polyester filament yarn. Compared with the prior art, the flame-retardant composite anchor rod provided by the invention is prepared from raw materials with specific content of components, so that the overall better interaction is realized, the product has excellent flame-retardant property on the basis of stable performance of various kinds, the safety of the anchor rod in the construction process is improved, and the flame-retardant composite anchor rod can be used in the fields with higher requirements on construction environment, such as coal mine tunnels and the like.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a flame-retardant composite anchor rod which is prepared from the following raw materials:
150-152 parts by weight of a fiber reinforcement material;
1000 parts by weight of unsaturated polyester resin;
5-9 parts of curing agent;
2-6 parts of styrene;
10 to 24 parts by weight of calcined kaolin;
0.5 to 1.5 parts by weight of cobalt iso-octoate;
80-300 parts by weight of halogen flame retardant;
5-6 parts of polyester filament yarn.
In the present invention, the fibrous reinforcement is preferably selected from basalt fibers and/or glass fibers, more preferably basalt fibers; the source of the fiber reinforced material is not particularly limited in the present invention, and commercially available basalt fiber roving and glass fiber roving known to those skilled in the art may be used.
In the present invention, the fiber diameter of the fiber-reinforced material is preferably 10 μm to 20 μm, more preferably 13 μm to 17 μm, the tensile strength is preferably 0.1N/tex or more, more preferably 0.3N/tex or more, the water content is preferably 0.5% or less, more preferably 0.1% or less, and the combustible content is preferably 0.1% to 1%, more preferably 0.0.25% to 0.65%.
In the present invention, the solid content of the unsaturated polyester resin is preferably 60% to 75%, more preferably 65% to 70%, the resin viscosity is preferably 300mpa.s to 1000mpa.s, more preferably 400mpa.s to 900mpa.s, and the acid value is preferably 10mg KOH/g to 30mg KOH/g, more preferably 14mg KOH/g to 22mg KOH/g; commercially available products satisfying the above-mentioned limitations and parameters, which are well known to those skilled in the art, may be used.
In the invention, the curing agent is preferably prepared from the following components in a mass ratio of (2-4): (1-3): 2, benzoyl peroxide and bis (4-tert-butylcyclohexyl) peroxydicarbonate), more preferably a mixture of 3: 2: 2 tert-butyl peroxybenzoate, benzoyl peroxide and bis (4-tert-butylcyclohexyl) peroxydicarbonate). The source of the curing agent is not particularly limited in the present invention, and commercially available products of the above-mentioned t-butyl peroxybenzoate, benzoyl peroxide and bis (4-t-butylcyclohexyl) peroxydicarbonate) known to those skilled in the art may be used.
In the present invention, the calcined kaolin is preferably 6000 mesh calcined kaolin, which is commercially available and well known to those skilled in the art.
In a preferred embodiment of the invention, the halogen flame retardant is prepared from (50-52) by mass: (30-32), wherein the flame-retardant composite material anchor rod comprises 80-84 parts by weight of halogen flame retardant, namely:
50-52 parts of decabromodiphenylethane;
30-32 parts of antimony trioxide;
preferably:
51 parts by weight of decabromodiphenylethane;
31 parts of antimony trioxide.
In another preferred embodiment of the present invention, the halogen flame retardant is a halogen flame retardant SZ 182, and in this case, the flame retardant composite anchor rod includes 200 to 300 parts by weight of the halogen flame retardant, that is, includes:
the halogen flame retardant SZ 182200 is preferably 250 parts by weight to 300 parts by weight.
In the invention, the polyester filament yarns can be 5000D polyester filament yarns and 8000D polyester filament yarns, and preferably 5000D polyester filament yarns.
The invention also provides a preparation method of the flame-retardant composite material anchor rod, which comprises the following steps:
a) mixing unsaturated polyester resin, a curing agent, styrene, calcined kaolin, cobalt isooctanoate and a halogen flame retardant to obtain a resin mixed material;
b) and b) dipping the fiber reinforced material by adopting the resin mixed material obtained in the step a), winding polyester filament yarns, and curing and forming to obtain the flame-retardant composite anchor rod.
In the present invention, the unsaturated polyester resin, the curing agent, the styrene, the calcined kaolin, the cobalt iso-octoate, the halogen flame retardant, the fiber reinforcement material and the polyester filament yarn are the same as those in the above technical solution, and are not described herein again.
The preparation method comprises the steps of firstly mixing unsaturated polyester resin, a curing agent, styrene, calcined kaolin, cobalt isooctanoate and a halogen flame retardant to obtain a resin mixed material. In the present invention, the mixing process preferably includes:
uniformly mixing a curing agent and styrene to obtain a curing agent mixture; then under the condition of low-speed stirring adding the above-mentioned solidifying agent mixture into unsaturated polyester resin; and then sequentially adding calcined kaolin, cobalt iso-octoate and halogen flame retardant, and stirring at a high speed to obtain a resin mixed material.
In the invention, the rotation speed of the low-speed stirring is preferably 100 r/min-200 r/min, and more preferably 150 r/min; the rotation speed of the high-speed stirring is preferably 500r/min to 600r/min, and more preferably 550 r/min. In the invention, the high-speed stirring temperature is preferably 10-35 ℃, and more preferably 25 ℃; the high-speed stirring time is preferably 10min to 25min, and more preferably 15 min.
In the invention, the viscosity of the resin mixture can reach 1000 mPa.S-1200 mPa.S.
After the resin mixture is obtained, the fiber reinforced material is dipped by the obtained resin mixture, and then the polyester filament yarns are wound, and the flame-retardant composite material anchor rod is obtained after curing and forming.
In the present invention, before the impregnation of the fiber reinforced material, it is preferable that the method further comprises:
and (6) threading and drawing yarns.
In the present invention, the process of threading and drawing is preferably as follows:
placing the fiber reinforced materials on a creel in sequence; during threading, the fiber reinforced material sequentially passes through the yarn arranging plates on the creel and then sequentially passes through the corresponding preforming plates, the impregnation tank and the mold; according to the specification of the anchor rod, selecting a proper yarn number for threading and drawing, and then manually drawing the yarn to pull the fiber reinforced material into the oven, and then passing through the fan cooling area and the water bath cooling area to the tractor.
In the present invention, the dipping process preferably includes:
pouring the resin mixed material into a glue tank, and uniformly dipping the fiber reinforced material which is arranged orderly into the resin mixed material; in the whole impregnation process, the fiber reinforced material is kept to be arranged neatly; the rubber content of the anchor rod is controlled by tightening the rubber extruding roller of the rubber groove, so that the rubber content is controlled to be 15-25%, and preferably 20-22%.
In the present invention, the process of winding the polyester filament yarn is preferably as follows:
winding the impregnated fiber reinforced material in a winding area, winding the polyester filament yarn on the fiber reinforced material through a winding device, controlling the tension to be 2 Hz-2.5 Hz, and ensuring the uniform thread pitch.
In the invention, the curing process is preferably carried out by adopting an oven, the oven is provided with 7 temperature zones, wherein the temperature zones are 340-360 ℃, 290-310 ℃, 240-260 ℃, 230-250 ℃, 220-240 ℃, 190-210 ℃ in sequence, and the heating time is preferably 5-6 min. By adopting the curing process, the fiber reinforced material and the matrix resin can be combined together through a crosslinking reaction at a high temperature, the anchor rod can be ensured to be cured after coming out of the heating oven, and the anchor rod has high strength and excellent mechanical structure after being cured.
In the present invention, after the curing, it is preferable to further include:
and (5) unwinding.
In the present invention, the unwinding process is preferably embodied as follows:
the terylene filament yarn is withdrawn in the withdrawal area, and the withdrawal speed, the winding speed and the traction speed are completely matched and consistent through intelligent control adjustment, so that the stability of the technological process is ensured.
In the present invention, the forming process preferably includes cutting and thread trimming, and chamfering.
In the present invention, the cutting process is preferably specifically:
cutting the composite anchor rod according to a specified length; the cutting length is preferably 1400-2600 mm; cutting length data is input into the control system, and the automatic control system accurately cuts after the length of the anchor rod reaches.
In the present invention, the thread trimming and chamfering process preferably includes:
after the composite anchor rod is cut according to the specified length, the cut anchor rod is firstly put into the inlet of a thread trimming machine one by one, a front end traction device drives the anchor rod to be conveyed forwards to a trimming device, and the anchor rod is conveyed to the tail part of the thread trimming machine through a rear end traction device after passing through a trimming head; and (4) carrying out corner cutting treatment on one end of the trimmed anchor rod.
The composite material anchor rod is a fiber reinforced resin matrix composite material prepared by taking epoxy resin, vinyl resin and the like as matrix materials and high-performance fibers (such as glass fibers, basalt fibers, aramid fibers, ultra-high molecular weight polyethylene fibers, carbon fibers and the like) as reinforcing materials and adopting a pultrusion process. According to the standard requirements of coal mines, the length of the composite anchor rod after cutting is generally between 1.4 and 2.6m, and the nominal diameter is between 18 and 32 mm. The flame-retardant composite material anchor rod provided by the invention adopts a specific formula and a production process (comprising steps, conditions and parameters), so that the flame-retardant property of the anchor rod is greatly improved, the flame-retardant capability of the product meets the standard requirement of a coal mine, the anchor rod can be used in the fields with higher construction environment requirements, such as coal mine roadways and the like, and the safety of the anchor rod construction process is improved.
The invention provides a flame-retardant composite anchor rod which is prepared from the following raw materials: 150-152 parts by weight of a fiber reinforcement material; 1000 parts by weight of unsaturated polyester resin; 5-9 parts of curing agent; 2-6 parts of styrene; 10 to 24 parts by weight of calcined kaolin; 0.5 to 1.5 parts by weight of cobalt iso-octoate; 80-300 parts by weight of halogen flame retardant; 5-6 parts of polyester filament yarn. Compared with the prior art, the flame-retardant composite anchor rod provided by the invention is prepared from raw materials with specific content of components, so that the overall better interaction is realized, the product has excellent flame-retardant property on the basis of stable performance of various kinds, the safety of the anchor rod in the construction process is improved, and the flame-retardant composite anchor rod can be used in the fields with higher requirements on construction environment, such as coal mine tunnels and the like.
To further illustrate the present invention, the following examples are provided for illustration. The raw materials used in the following examples of the present invention are all commercially available products; wherein, the fiber diameter of the basalt fiber is: 15 ± 2 μm, tensile strength: not less than 0.3N/tex, water content: less than or equal to 0.1 percent and combustible content: (0.45 ± 0.2)%; solid content of unsaturated polyester resin: (65-70)%, resin viscosity: 400-900 mPa.S, acid value: 14 to 22mg KOH/g.
Example 1
The formula of the flame-retardant composite anchor rod comprises the following components:
150-152 parts of basalt fiber untwisted roving;
1000 parts by weight of unsaturated polyester resin;
3 parts by weight of tert-butyl peroxybenzoate (the purity is more than or equal to 99 percent);
2 parts by weight of benzoyl peroxide (purity 74%);
2 parts by weight of a special rapid curing agent (di (4-tert-butylcyclohexyl) peroxydicarbonate) for pultrusion;
4 parts by weight of styrene;
11 parts by weight of calcined kaolin (6000 meshes);
1 part by weight of cobalt isooctanoate (cobalt content is 8 +/-0.2%);
51 parts of decabromodiphenylethane (the bromine content is more than or equal to 81 percent);
31 parts of antimony trioxide (the whiteness is more than or equal to 98%);
5-6 parts of polyester filament yarn.
The preparation method of the 22mm flame-retardant composite anchor rod comprises the following steps:
s1: threading and drawing yarn
Placing basalt fiber yarns on a creel, and placing the basalt fiber yarns in sequence; when threading, the yarn sequentially passes through the yarn arranging plates on the creel and then sequentially passes through the corresponding preforming plates, the impregnation tank and the mold; according to the specification of the anchor rod, selecting a proper yarn number for threading and drawing, wherein the total yarn number of the anchor rod with the specification of 22mm is divided into a central yarn and a peripheral yarn, wherein 80-82 fiber yarns with the linear density of 4800tex are selected as the central yarn, and 30-32 fiber yarns with the linear density of 4800tex are selected as the peripheral yarn; and (4) subsequently, manually drawing the yarns to pull the fiber yarns into the oven, and then, passing through the fan cooling area and the water bath cooling area to the tractor.
S2: resin mixing
Weighing the components of the formula, namely unsaturated polyester resin, tert-butyl peroxybenzoate, benzoyl peroxide, a special rapid curing agent for pultrusion, styrene, calcined kaolin, cobalt iso-octoate, decabromodiphenylethane and antimony trioxide, by using an electronic balance according to the formula, and putting the materials into a stirring tank for stirring according to the feeding sequence after weighing; the material preparation sequence is as follows: firstly, weighing unsaturated polyester resin, placing the unsaturated polyester resin in a mixing barrel, placing the unsaturated polyester resin under a stirrer, starting to stir at a low speed (150r/min), uniformly mixing benzoyl peroxide, a special rapid curing agent for pultrusion, tert-butyl peroxybenzoate and styrene in a glass cup in advance, and then slowly pouring the mixed curing agent into the mixing barrel of the unsaturated polyester resin during stirring; then adding calcined kaolin, dripping cobalt iso-octoate by using a rubber head dropper, finally adding decabromodiphenylethane and antimony trioxide, increasing the stirring speed to 550r/min, controlling the stirring temperature to be about 25 ℃, and stirring for 15 minutes; if the temperature in summer exceeds 30 ℃, the stirring time is reduced to 12 minutes; when the temperature is lower than 15 ℃ in winter, the stirring time is prolonged to 20 minutes; and then, after the resin is clear and transparent, ending stirring, and measuring the viscosity of the mixture by using a viscometer, wherein the viscosity of the mixture can reach 1000-1200 mPa.S for use.
S3: impregnation
Pouring the mixed resin mixture into a glue tank, and uniformly dipping the fiber yarns which are arranged orderly into the prepared resin mixture; in the whole impregnation process, the arrangement of the yarns must be ensured to be very regular; the rubber content of the anchor rod is controlled by tightening the rubber extruding roller of the rubber groove, so that the rubber content is controlled to be 20-22%.
S4: winding of
Setting the traction speed to be 1.5m/min, the winding tension to be 30-31 Hz, the winding torque to be 1.5-1.6 Hz, and setting the thread pitch of the flame-retardant composite anchor rod to be 10 mm; winding the impregnated fiber yarn in a winding area, and winding a winding wire (adopting a 5000D polyester filament yarn) through a winding device to wind the fiber yarn, so as to ensure uniform thread pitch; the winding area is provided with a precise winding device, the tightness degree of the tension wheel is controllable, so that the tension is adjusted, the tension is controlled at 2-2.5 Hz, the tension is controlled uniformly in the winding process, the controllability is good, and the thread of the anchor rod is stable in production.
S5: curing
Heating the resin-impregnated anchor rod fiber yarns through a heating oven, wherein the heating time is controlled to be 5-6 minutes, so that the reinforced fiber yarns and the matrix resin can be combined together through a crosslinking reaction at a high temperature, the anchor rod can be ensured to be cured after the reinforced fiber yarns and the matrix resin are taken out of the heating oven, the strength after curing is high, and the mechanical structure is excellent; the curing zone has seven temperature zones, and the temperature is shown in table 1.
TABLE 1 oven temperature for producing 22mm flame-retardant composite anchor rod
| Temperature zone | A region | Two zones | Three zones | Four zones | Five zones | Six zones | Seven regions |
| Temperature (. degree.C.) | 350±10 | 300±10 | 250±10 | 240±10 | 230±10 | 230±10 | 200±10 |
S6: backing-off
The winding wire can be withdrawn in the unwinding area through the preheated anchor rod, and the unwinding speed, the winding speed and the traction speed are completely matched and consistent through intelligent control adjustment, so that the stability of the technological process is ensured; the drawing speed was 1.5m/min and the unwinding speed was 150 r/min.
S7: cutting of
The composite anchor rod is cut according to the specified length, the general cutting length is controlled to be 1400-2600 mm, the cutting length data is input into a control system, and the anchor rod is accurately cut by an automatic control system after the length of the anchor rod reaches.
S8: thread trimming and chamfering
After the composite anchor rod is cut according to the specified length, the cut anchor rod is firstly put into the inlet of a thread trimming machine one by one, a front end traction device drives the anchor rod to be conveyed forwards to a trimming device, and the anchor rod is conveyed to the tail part of the thread trimming machine through a rear end traction device after passing through a trimming head; and (4) carrying out corner cutting treatment on one end of the trimmed anchor rod to obtain the 22mm flame-retardant composite anchor rod.
Example 2
Obtaining a 22mm flame-retardant composite anchor rod by adopting the preparation method provided by the embodiment 1; the difference lies in that:
the formula of the flame-retardant composite anchor rod in the embodiment 2 is as follows:
150-152 parts of basalt fiber untwisted roving;
1000 parts by weight of unsaturated polyester resin;
3 parts by weight of tert-butyl peroxybenzoate (the purity is more than or equal to 99 percent);
2 parts by weight of benzoyl peroxide (purity 74%);
2 parts by weight of a special rapid curing agent (di (4-tert-butylcyclohexyl) peroxydicarbonate) for pultrusion;
4 parts by weight of styrene;
22 parts by weight of calcined kaolin (6000 meshes);
1 part by weight of cobalt isooctanoate (cobalt content is 8 +/-0.2%);
250 parts by weight of halogen flame retardant SZ 182 (the halogen content is more than or equal to 80%);
5-6 parts of polyester filament yarn.
The performances of the flame-retardant composite anchor rod obtained by the preparation method provided by the embodiments 1-2 of the invention are detected, and the results are shown in tables 2-6.
Table 2 flame burning time of the flame retardant composite anchor rod obtained by the preparation method provided in embodiment 1 of the present invention
Table 3 flameless combustion time of the flame retardant composite anchor rod obtained by the preparation method provided in embodiment 1 of the present invention
Table 4 flame burning time of the flame retardant composite anchor rod obtained by the preparation method provided in embodiment 2 of the present invention
Table 5 flameless combustion time of the flame retardant composite anchor rod obtained by the preparation method provided in embodiment 2 of the present invention
Table 6 mechanical property data of the flame retardant composite anchor rod obtained by the preparation method provided in embodiments 1 to 2 of the present invention
| Rod diameter (mm) | Technical index | Example 1 | Example 2 |
| Tensile strength (MPa) | ≥300 | 525 | 508 |
| Shear strength (MPa) | ≥75 | 105 | 100 |
| Torque (N.M) | ≥40 | 48 | 50 |
| Anchoring force (KN) | ≥60 | 75 | 78 |
| Bearing capacity of tray and nut (KN) | ≥60 | 81 | 77 |
Experimental results show that the flame-retardant composite anchor rod obtained by the preparation method provided by the invention has excellent flame-retardant performance on the basis of stable performance of various kinds, and meets mining standards.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A flame-retardant composite anchor rod is prepared from the following raw materials:
150-152 parts by weight of a fiber reinforcement material;
1000 parts by weight of unsaturated polyester resin;
5-9 parts of curing agent;
2-6 parts of styrene;
10 to 24 parts by weight of calcined kaolin;
0.5 to 1.5 parts by weight of cobalt iso-octoate;
80-300 parts by weight of halogen flame retardant;
5-6 parts of polyester filament yarn.
2. A fire retardant composite bolt according to claim 1, characterised in that the fibrous reinforcement is selected from basalt fibres and/or glass fibres; the fiber diameter of the fiber reinforced material is 10-20 μm, the tensile strength is more than or equal to 0.1N/tex, the water content is less than or equal to 0.5%, and the content of combustible is 0.1-1%.
3. The flame-retardant composite anchor rod according to claim 1, wherein the unsaturated polyester resin has a solid content of 60 to 75%, a resin viscosity of 300 to 1000mpa.s, and an acid value of 10 to 30mg KOH/g.
4. The flame-retardant composite anchor rod according to claim 1, wherein the curing agent is prepared from the following components in percentage by mass (2-4): (1-3): 2 tert-butyl peroxybenzoate, benzoyl peroxide and bis (4-tert-butylcyclohexyl) peroxydicarbonate).
5. The flame-retardant composite anchor rod according to claim 1, wherein the halogen flame retardant is prepared from the following components in a mass ratio of (50-52): (30-32) decabromodiphenylethane and antimony trioxide,
or, the halogen flame retardant SZ 182.
6. A method for preparing a flame-retardant composite anchor rod according to any one of claims 1 to 5, comprising the steps of:
a) mixing unsaturated polyester resin, a curing agent, styrene, calcined kaolin, cobalt isooctanoate and a halogen flame retardant to obtain a resin mixed material;
b) and b) dipping the fiber reinforced material by adopting the resin mixed material obtained in the step a), winding polyester filament yarns, and curing and forming to obtain the flame-retardant composite anchor rod.
7. The method according to claim 6, wherein the mixing in step a) is carried out by:
uniformly mixing a curing agent and styrene to obtain a curing agent mixture; then under the condition of low-speed stirring adding the above-mentioned solidifying agent mixture into unsaturated polyester resin; then sequentially adding calcined kaolin, cobalt iso-octoate and halogen flame retardant, and stirring at a high speed to obtain a resin mixed material; the rotating speed of the low-speed stirring is 100 r/min-200 r/min; the high-speed stirring speed is 500 r/min-600 r/min, the temperature is 10-35 ℃, and the time is 10-25 min.
8. The preparation method according to claim 6, wherein the dipping in step b) is carried out by:
pouring the resin mixed material into a glue tank, and uniformly dipping the fiber reinforced material which is arranged orderly into the resin mixed material; in the whole impregnation process, the fiber reinforced material is kept to be arranged neatly; the rubber content of the anchor rod is controlled by the tightening of the rubber extruding roller of the rubber groove, so that the rubber content is controlled to be 15-25%.
9. The method according to claim 6, wherein the step b) of winding the polyester filament yarn comprises:
winding the impregnated fiber reinforced material in a winding area, winding the polyester filament yarn on the fiber reinforced material through a winding device, controlling the tension to be 2 Hz-2.5 Hz, and ensuring the uniform thread pitch.
10. The preparation method of claim 6, wherein the curing process in step b) is performed by using an oven, and the oven has 7 temperature zones, which are 340-360 ℃, 290-310 ℃, 240-260 ℃, 230-250 ℃, 220-240 ℃, 190-210 ℃ in sequence, and the heating time is 5-6 min.
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