CN108587117A - A kind of hydraulic engineering grouting flame retardant polyurethane compositions and preparation method thereof - Google Patents
A kind of hydraulic engineering grouting flame retardant polyurethane compositions and preparation method thereof Download PDFInfo
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- CN108587117A CN108587117A CN201810514979.2A CN201810514979A CN108587117A CN 108587117 A CN108587117 A CN 108587117A CN 201810514979 A CN201810514979 A CN 201810514979A CN 108587117 A CN108587117 A CN 108587117A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
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- 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
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Soil Conditioners And Soil-Stabilizing Materials (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a kind of hydraulic engineering grouting flame retardant polyurethane compositions and preparation method thereof.The flame retardant polyurethane compositions include the raw material of following parts by weight：105 150 parts of aqueous polyurethane, 11 15 parts of nickel nitrate, 13 18 parts of carbohydrazide, 8 15 parts of polyethylene glycol stearate, 6 13 parts of 4 hydroxyphenethylamine, 6 15 parts of chlorogenic acid, 26 parts of barbiturates.The hydraulic engineering grouting of the present invention is that primary raw material is combined by aqueous polyurethane, nickel nitrate, carbohydrazide, polyethylene glycol stearate, 4 hydroxyphenethylamines, chlorogenic acid and barbiturates with flame retardant polyurethane compositions, it is more environment-friendly and safer using water as solvent；Have many advantages, such as that good flame retardation effect, setting time are short, intensity is high；Preparation process is simple, is advantageously implemented industrialized production.
Description
Technical field
The present invention relates to hydraulic engineering technical field, specifically a kind of hydraulic engineering grouting flame retardant polyurethane compositions and
Preparation method.
Background technology
Polyurethane grouting material has been more and more widely used because of its superior performance in the engineerings such as water conservancy, water power,
Strengthening of foundation, leak stopping sealing, curtain especially in engineering construction are prevented blending crack repairing etc..But in the prior art
Polyurethane grouting material is required to that the low-flashes flammable solvents such as acetone, dimethylbenzene are added and poisons big plasticising to environment, human body
Agent is diluted, and improves the flowing diffusion of slurry material with this.Due to containing low-flash flammable liquid, general flash-point is below 61
DEG C, therefore it is very high to the fire protection requirement of construction site, it is careless slightly to lead to major accident.Furthermore due to these solvents,
Plasticizer itself has stronger volatility and toxicity, and the personnel health in engineering is constituted and is greatly threatened.It is domestic simultaneously
Flammable liquid transport standard is required high, special hazardous materials transportation vehicle is needed to transport, undoubtedly increase the operation of enterprise at
This, and it is potential dangerous also big.
Invention content
The purpose of the present invention is to provide a kind of hydraulic engineering grouting flame retardant polyurethane compositions and preparation method thereof, with
Solve the problems mentioned above in the background art.
To achieve the above object, the present invention provides the following technical solutions：
A kind of hydraulic engineering grouting flame retardant polyurethane compositions, the flame retardant polyurethane compositions include following parts by weight
Several raw materials：105-150 parts of aqueous polyurethane, 11-15 parts of nickel nitrate, 13-18 parts of carbohydrazide, polyethylene glycol stearate 8-15
Part, 6-13 parts of 4- hydroxyphenethylamines, 6-15 parts of chlorogenic acid, 2-6 parts of barbiturates.
As a further solution of the present invention：The flame retardant polyurethane compositions include the raw material of following parts by weight：Water
112-135 parts of polyurethane of property, 12-14 parts of nickel nitrate, 15-17 parts of carbohydrazide, 10-13 parts of polyethylene glycol stearate, 4- hydroxyls
8-12 parts of phenyl ethylamine, 9-13 parts of chlorogenic acid, 3-5 parts of barbiturates.
As a further solution of the present invention：The flame retardant polyurethane compositions include the raw material of following parts by weight：Water
It is 126 parts of polyurethane of property, 13 parts of nickel nitrate, 16 parts of carbohydrazide, 11 parts of polyethylene glycol stearate, 10 parts of 4- hydroxyphenethylamines, green
11 parts of ortho acid, 4 parts of barbiturates.
A kind of preparation method of hydraulic engineering grouting flame retardant polyurethane compositions, includes the following steps：
(1) nickel nitrate and carbohydrazide are mixed, the water of 2-7 times of mixture is added, turned with 100-250r/min at 60-75 DEG C
Speed is stirred 10-20min；
(2) aqueous polyurethane and upper step gains are mixed, 5- is stirred with rotating speed 800-1000r/min at 50-60 DEG C
10min；Then it is slowly added to 4- hydroxyphenethylamines thereto, 2-5min is stirred with rotating speed 1500-2000r/min, is then heated up
To 82-90 DEG C, 5-7min is kept the temperature；
(3) chlorogenic acid and barbiturates are mixed, the water of 2-7 times of mixture is added, at 25-40 DEG C with 300-550r/min
Rotating speed is stirred 5-10min；
(4) step (2) gains and step (3) gains are mixed, at 90-100 DEG C with rotating speed 1500-2000r/min
Stir 2-4min；Then it is slowly added to polyethylene glycol stearate thereto, 5-8min is stirred with rotating speed 2200-2500r/min,
90-98 DEG C is then heated to, 3-5min is kept the temperature；Be down to room temperature to get.
As a further solution of the present invention：Step (1) mixes nickel nitrate and carbohydrazide, and the water of 5 times of mixture is added,
14min is stirred with 185r/min rotating speeds at 68 DEG C.
As a further solution of the present invention：Step (2) mixes aqueous polyurethane and upper step gains, at 56 DEG C to turn
Fast 900r/min stirs 8min；Then it is slowly added to 4- hydroxyphenethylamines thereto, 3min is stirred with rotating speed 1700r/min, so
After be warming up to 88 DEG C, keep the temperature 6min.
As a further solution of the present invention：Step (3) mixes chlorogenic acid and barbiturates, and 4 times of mixture is added
Water is stirred 7min at 35 DEG C with 450r/min rotating speeds.
As a further solution of the present invention：Step (4) mixes step (2) gains and step (3) gains, 95
DEG C 3min is stirred with rotating speed 1700r/min；Then it is slowly added to polyethylene glycol stearate thereto, with rotating speed 2400r/min
6min is stirred, then heats to 94 DEG C, keeps the temperature 4min；Be down to room temperature to get.
Compared with prior art, the beneficial effects of the invention are as follows：
The hydraulic engineering grouting flame retardant polyurethane compositions of the present invention pass through aqueous polyurethane, nickel nitrate, carbohydrazide, poly-
Ethylene glycol stearate, 4- hydroxyphenethylamines, chlorogenic acid and barbiturates are combined for primary raw material, produce unexpected
Synergistic effect, it is more environment-friendly and safer using water as solvent；Have many advantages, such as that good flame retardation effect, setting time are short, intensity is high；
Preparation process is simple, is advantageously implemented industrialized production.
Specific implementation mode
The technical solution of this patent is described in more detail With reference to embodiment.
Embodiment 1
A kind of hydraulic engineering grouting flame retardant polyurethane compositions, the flame retardant polyurethane compositions include following parts by weight
Several raw materials：105 parts of aqueous polyurethane, 11 parts of nickel nitrate, 13 parts of carbohydrazide, 8 parts of polyethylene glycol stearate, 4- hydroxy benzenes second
6 parts of amine, 6 parts of chlorogenic acid, 2 parts of barbiturates.
A kind of preparation method of hydraulic engineering grouting flame retardant polyurethane compositions, includes the following steps：(1) by nickel nitrate
It is mixed with carbohydrazide, the water of 2 times of mixture is added, 10min is stirred with 100r/min rotating speeds at 60 DEG C；It (2) will be aqueous poly-
Urethane and the mixing of upper step gains, 5min is stirred at 50 DEG C with rotating speed 800r/min；Then it is slowly added to 4- hydroxy benzenes thereto
Ethamine stirs 2min with rotating speed 1500r/min, then heats to 82 DEG C, keeps the temperature 5min；(3) chlorogenic acid and barbiturates are mixed
It closes, the water of 2 times of mixture is added, 5min is stirred with 300r/min rotating speeds at 25 DEG C；(4) by step (2) gains and step
Suddenly (3) gains mix, and 2min is stirred with rotating speed 1500r/min at 90 DEG C；Then it is slowly added to polyethylene glycol tristearin thereto
Acid esters stirs 5min with rotating speed 2200r/min, then heats to 90 DEG C, keeps the temperature 3min；Be down to room temperature to get.
Embodiment 2
A kind of hydraulic engineering grouting flame retardant polyurethane compositions, the flame retardant polyurethane compositions include following parts by weight
Several raw materials：150 parts of aqueous polyurethane, 15 parts of nickel nitrate, 18 parts of carbohydrazide, Solutol HS15 part, 4- hydroxy benzenes
13 parts of ethamine, 15 parts of chlorogenic acid, 6 parts of barbiturates.
A kind of preparation method of hydraulic engineering grouting flame retardant polyurethane compositions, includes the following steps：(1) by nickel nitrate
It is mixed with carbohydrazide, the water of 7 times of mixture is added, 20min is stirred with 250r/min rotating speeds at 75 DEG C；It (2) will be aqueous poly-
Urethane and the mixing of upper step gains, 10min is stirred at 60 DEG C with rotating speed 1000r/min；Then it is slowly added to 4- hydroxyls thereto
Phenyl ethylamine stirs 5min with rotating speed 2000r/min, then heats to 90 DEG C, keeps the temperature 7min；(3) by chlorogenic acid and barbiturates
Mixing is added the water of 7 times of mixture, 10min is stirred with 550r/min rotating speeds at 40 DEG C；(4) by step (2) gains and
Step (3) gains mix, and 4min is stirred with rotating speed 2000r/min at 100 DEG C；Then it is hard that it is slowly added to polyethylene glycol thereto
Resin acid ester stirs 8min with rotating speed 2500r/min, then heats to 98 DEG C, keeps the temperature 5min；Be down to room temperature to get.
Embodiment 3
A kind of hydraulic engineering grouting flame retardant polyurethane compositions, the flame retardant polyurethane compositions include following parts by weight
Several raw materials：126 parts of aqueous polyurethane, 13 parts of nickel nitrate, 16 parts of carbohydrazide, 11 parts of polyethylene glycol stearate, 4- hydroxy benzenes
10 parts of ethamine, 11 parts of chlorogenic acid, 4 parts of barbiturates.
A kind of preparation method of hydraulic engineering grouting flame retardant polyurethane compositions, includes the following steps：(1) by nickel nitrate
It is mixed with carbohydrazide, the water of 5 times of mixture is added, 14min is stirred with 185r/min rotating speeds at 68 DEG C.It (2) will be aqueous poly-
Urethane and the mixing of upper step gains, 8min is stirred at 56 DEG C with rotating speed 900r/min；Then it is slowly added to 4- hydroxy benzenes thereto
Ethamine stirs 3min with rotating speed 1700r/min, then heats to 88 DEG C, keeps the temperature 6min.(3) chlorogenic acid and barbiturates are mixed
It closes, the water of 4 times of mixture is added, 7min is stirred with 450r/min rotating speeds at 35 DEG C.(4) by step (2) gains and step
Suddenly (3) gains mix, and 3min is stirred with rotating speed 1700r/min at 95 DEG C；Then it is slowly added to polyethylene glycol tristearin thereto
Acid esters stirs 6min with rotating speed 2400r/min, then heats to 94 DEG C, keeps the temperature 4min；Be down to room temperature to get.
Embodiment 4
A kind of hydraulic engineering grouting flame retardant polyurethane compositions, the flame retardant polyurethane compositions include following parts by weight
Several raw materials：112 parts of aqueous polyurethane, 12 parts of nickel nitrate, 15 parts of carbohydrazide, 10 parts of polyethylene glycol stearate, 4- hydroxy benzenes
8 parts of ethamine, 9 parts of chlorogenic acid, 3 parts of barbiturates.
A kind of preparation method of hydraulic engineering grouting flame retardant polyurethane compositions, includes the following steps：(1) by nickel nitrate
It is mixed with carbohydrazide, the water of 3 times of mixture is added, 12min is stirred with 125r/min rotating speeds at 62 DEG C；It (2) will be aqueous poly-
Urethane and the mixing of upper step gains, 6min is stirred at 53 DEG C with rotating speed 850r/min；Then it is slowly added to 4- hydroxy benzenes thereto
Ethamine stirs 2.5min with rotating speed 1600r/min, then heats to 86 DEG C, keeps the temperature 6.2min；(3) by chlorogenic acid and barbital
Acid mixing, is added the water of 3 times of mixture, 6min is stirred with 370r/min rotating speeds at 26 DEG C；(4) by step (2) gains
It is mixed with step (3) gains, 2.4min is stirred with rotating speed 1600r/min at 93 DEG C；Then it is slowly added to poly- second two thereto
Alcohol stearate stirs 6min with rotating speed 2250r/min, then heats to 92 DEG C, keeps the temperature 3.5min；Be down to room temperature to get.
Embodiment 5
A kind of hydraulic engineering grouting flame retardant polyurethane compositions, the flame retardant polyurethane compositions include following parts by weight
Several raw materials：135 parts of aqueous polyurethane, 14 parts of nickel nitrate, 17 parts of carbohydrazide, 13 parts of polyethylene glycol stearate, 4- hydroxy benzenes
12 parts of ethamine, 13 parts of chlorogenic acid, 5 parts of barbiturates.
A kind of preparation method of hydraulic engineering grouting flame retardant polyurethane compositions, includes the following steps：(1) by nickel nitrate
It is mixed with carbohydrazide, the water of 6 times of mixture is added, 17min is stirred with 230r/min rotating speeds at 72 DEG C；It (2) will be aqueous poly-
Urethane and the mixing of upper step gains, 8min is stirred at 58 DEG C with rotating speed 900r/min；Then it is slowly added to 4- hydroxy benzenes thereto
Ethamine stirs 4min with rotating speed 1800r/min, then heats to 88 DEG C, keeps the temperature 6.5min；(3) by chlorogenic acid and barbiturates
Mixing is added the water of 6 times of mixture, 8min is stirred with 500r/min rotating speeds at 36 DEG C；(4) by step (2) gains and
Step (3) gains mix, and 3.5min is stirred with rotating speed 1900r/min at 97 DEG C；Then it is slowly added to polyethylene glycol thereto
Stearate stirs 7min with rotating speed 2450r/min, then heats to 96 DEG C, keeps the temperature 4.5min；Be down to room temperature to get.
Comparative example 1
Compared with Example 3, in addition to not containing carbohydrazide in raw material, other preparation processes are consistent.
Comparative example 2
Compared with Example 3, in addition to not containing 4- hydroxyphenethylamines in raw material, other preparation processes are consistent.
Comparative example 3
Compared with Example 3, in addition to not containing carbohydrazide and 4- hydroxyphenethylamines in raw material, other preparation processes are consistent.
Comparative example 4
Compared with Example 3, raw material is identical, preparation process be by all raw materials together be uniformly mixed to get.
Experimental example
Embodiment 1-3 and comparative example 1-4 are tested for the property.Reference standard：JC/T2041-2010；GB8323-
2008；GB/T5455-1997；GB/T5454-1997 etc..Test result see the table below shown：
1 test result of table
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Non-volatile content % | 99.1 | 99.0 | 99.6 | 92.3 | 93.1 | 90.2 | 95.6 |
| Setting time s | 122 | 112 | 105 | 280 | 251 | 355 | 158 |
| Compression strength MPa | 14 | 16 | 18 | 10 | 11 | 8 | 13 |
| Adhesion strength MPa | 0.61 | 0.58 | 0.67 | 0.35 | 0.38 | 0.31 | 0.52 |
| Tensile strength MPa | 0.98 | 0.96 | 0.99 | 0.68 | 0.71 | 0.63 | 0.89 |
| Elongation at break % | 185 | 192 | 205 | 159 | 161 | 140 | 168 |
| Maximum smoke density | 11 | 14 | 10 | 20 | 18 | 22 | 13 |
| Oxygen index (OI) | 28.9 | 29.6 | 31.1 | 24.3 | 24.2 | 23.7 | 20.9 |
| Flaming combustion time/s | 11.3 | 9.9 | 6.7 | 17.8 | 15.6 | 19.7 | 14.5 |
| Glowing time/s | 0 | 0.1 | 0 | 0.7 | 0.5 | 0.9 | 0.3 |
The better embodiment of this patent is explained in detail above, but this patent is not limited to above-mentioned embodiment party
Formula, one skilled in the relevant art within the scope of knowledge, can also be under the premise of not departing from this patent objective
Various changes can be made.
Claims (8)
1. a kind of hydraulic engineering grouting flame retardant polyurethane compositions, which is characterized in that the flame retardant polyurethane compositions include
The raw material of following parts by weight：105-150 parts of aqueous polyurethane, 11-15 parts of nickel nitrate, 13-18 parts of carbohydrazide, polyethylene glycol are hard
8-15 parts of resin acid ester, 6-13 parts of 4- hydroxyphenethylamines, 6-15 parts of chlorogenic acid, 2-6 parts of barbiturates.
2. hydraulic engineering grouting flame retardant polyurethane compositions according to claim 1, which is characterized in that described fire-retardant poly-
Urethane composition includes the raw material of following parts by weight：112-135 parts of aqueous polyurethane, 12-14 parts of nickel nitrate, carbohydrazide 15-
17 parts, 10-13 parts of polyethylene glycol stearate, 8-12 parts of 4- hydroxyphenethylamines, 9-13 parts of chlorogenic acid, 3-5 parts of barbiturates.
3. hydraulic engineering grouting flame retardant polyurethane compositions according to claim 1, which is characterized in that described fire-retardant poly-
Urethane composition includes the raw material of following parts by weight：126 parts of aqueous polyurethane, 13 parts of nickel nitrate, 16 parts of carbohydrazide, poly- second two
11 parts of alcohol stearate, 10 parts of 4- hydroxyphenethylamines, 11 parts of chlorogenic acid, 4 parts of barbiturates.
4. a kind of preparation method according to any hydraulic engineering grouting flame retardant polyurethane compositions of claim 1-3,
It is characterized by comprising the following steps：
（1）Nickel nitrate and carbohydrazide are mixed, the water of 2-7 times of mixture is added, is stirred with 100-250r/min rotating speeds at 60-75 DEG C
Mix mixing 10-20min；
（2）Aqueous polyurethane and upper step gains are mixed, 5-10min is stirred with rotating speed 800-1000r/min at 50-60 DEG C；
Then it is slowly added to 4- hydroxyphenethylamines thereto, 2-5min is stirred with rotating speed 1500-2000r/min, then heats to 82-90
DEG C, keep the temperature 5-7min；
（3）Chlorogenic acid and barbiturates are mixed, the water of 2-7 times of mixture is added, at 25-40 DEG C with 300-550r/min rotating speeds
It is stirred 5-10min；
（4）By step（2）Gains and step（3）Gains mix, and are stirred with rotating speed 1500-2000r/min at 90-100 DEG C
2-4min；Then it is slowly added to polyethylene glycol stearate thereto, 5-8min is stirred with rotating speed 2200-2500r/min, then
It is warming up to 90-98 DEG C, keeps the temperature 3-5min；Be down to room temperature to get.
5. the preparation method of hydraulic engineering grouting flame retardant polyurethane compositions according to claim 4, which is characterized in that
Step（1）Nickel nitrate and carbohydrazide are mixed, the water of 5 times of mixture is added, is stirred with 185r/min rotating speeds at 68 DEG C
14min。
6. the preparation method of hydraulic engineering grouting flame retardant polyurethane compositions according to claim 4, which is characterized in that
Step（2）Aqueous polyurethane and upper step gains are mixed, 8min is stirred with rotating speed 900r/min at 56 DEG C；Then delay thereto
It is slow that 4- hydroxyphenethylamines are added, 3min is stirred with rotating speed 1700r/min, then heats to 88 DEG C, keeps the temperature 6min.
7. the preparation method of hydraulic engineering grouting flame retardant polyurethane compositions according to claim 4, which is characterized in that
Step（3）Chlorogenic acid and barbiturates are mixed, the water of 4 times of mixture is added, is stirred with 450r/min rotating speeds at 35 DEG C
7min。
8. the preparation method of hydraulic engineering grouting flame retardant polyurethane compositions according to claim 4, which is characterized in that
Step（4）By step（2）Gains and step（3）Gains mix, and 3min is stirred with rotating speed 1700r/min at 95 DEG C；Then
It is slowly added to polyethylene glycol stearate thereto, 6min is stirred with rotating speed 2400r/min, then heats to 94 DEG C, heat preservation
4min；Be down to room temperature to get.
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Application publication date: 20180928 |