CN101724413B - Retardant and preparation method thereof - Google Patents
Retardant and preparation method thereof Download PDFInfo
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- CN101724413B CN101724413B CN2008101679194A CN200810167919A CN101724413B CN 101724413 B CN101724413 B CN 101724413B CN 2008101679194 A CN2008101679194 A CN 2008101679194A CN 200810167919 A CN200810167919 A CN 200810167919A CN 101724413 B CN101724413 B CN 101724413B
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Abstract
The invention discloses retardant and a preparation method thereof, belonging to the field of retardant products. The retardant comprises the following compositions by weight part: 100 to 400 parts of calcium carbide waste residue, 130 to 500 parts of sulfamic acid, 10 to 90 parts of phosphoric acid, 50 to 200 parts of boric acid, 50 to 200 parts of borax, 0.2 to 5 parts of penetrant, 1 to 10 parts of polyol, 1 to 10 parts of surfactant, 1 to 10 parts of defoamer, 0.2 to 5 parts of sandalwood essence, and 150 to 600 parts of water. The retardant is prepared mainly by the calcium carbide waste residue, provides an effective utilization way for calcium carbide waste residue treatment, and has excellent retarding performance and low prices. The retardant can be widely applied to the preparation of artificial boards, wood materials, cotton cloth, paper and the like which have fire resistence.
Description
Technical field
The present invention relates to a kind of fire retardant, relate in particular to a kind of fire retardant that calcium carbide waste slag is prepared from and preparation method thereof that mainly utilizes, belong to field of flame retardant products.
Background technology
Acetylene is one of important source material of basic organic synthesis industry, and it is a raw material with the calcium carbide, adds water (wet method) production, and year history surplus in the of existing 60 still accounts for larger specific gravity in China at present so far.1 ton of calcium carbide adds water and can generate more than 300 kilogram of acetylene gas, but also generates the trade waste of 10 tons of solid contents about 12% simultaneously, is commonly called as carbide slag slurries, and its disposal makes manufacturer's headache always.
The calcium carbide waste slag and the percolate that contain certain water yield are strong basicity, contain poisonous, objectionable impuritiess such as sulfide, phosphide.According to " Hazardous wastes judging standard " (GB5085-1996); Calcium carbide waste slag belongs to II class general industry solid waste; If directly it is discharged in seawall or the mountain valley, when adopting and filling out the sea, filling out the regular stacking of ditch, according to " chemical sludge landfill yard design code " (HG20504-92); To useless (thing) slag of II class general industry solid, must take seepage control measure and do the landfill disposal.
Acetylene is the main raw material of producing PVC RESINS (PVC); Because 1 ton of PVC product of every production consumes about 1.5~1.6 tons of calcium carbide, calcium carbide simultaneously per ton produces 1.2 tons of carbide slags (butt), and the carbide slag water cut is by 90%; 1 ton of PVC product of so every production is then discharged about 20 tons of carbide slag slurries.This shows that the generation of carbide slag slurries has substantially exceeded the output of PVC.Most of PVC manufacturer with carbide slag slurries after gravity settling separation, the supernatant recycle; Carbide slag is through further dehydration, and its water ratio still reaches 40%~50%, is starchiness, and easy to leak pollutes the road surface in transit, and long-term accumulation not only takies a large amount of soils, and there is serious erosion action in the soil.Want to tackle the problem at its root, have only and seek technically to break through, seek new improvement technology, comprehensive utilization turns harm into good, and turns waste into wealth.
In China, also there is enterprise to utilize calcium carbide waste slag system cement, adopt concentration basin that slag is starched concentration and be concentrated to 35% by 5%~8%, send into hopper with sand pump,, branch, is mixed with cement slurry after removing a part of supernatant with sandstone, clay slip, send the rotary kiln calcine cement back to.The wet processing that is main raw material with general employing Wingdale compares, and the carbide slag water cut is high, and is mobile poor, so hear rate is generally high by about 20% than wet method.
Because it is high to go into kiln slurry moisture content, the regenerator section load of kiln is heavier, low 50~60 ℃ of the general wet production line of kiln discharge tail spent air temp, so the output of kiln is the production line low 20%~25% of batching with the Wingdale than same specification.In addition, Ca (OH)
2Produce water vapor during decomposition, cause water vapour content increase in the kiln tail gas, influence the service efficiency and the life-span of electric precipitator, so the cement that calcium carbide waste slag is produced is welcome not as the cement that Wingdale is produced in market.
At present; The PVC that calcium carbide route is produced accounts for 60% of China's output; Press 1 ton of PVC of every production and produce 1.59 tons of calcium carbide slag cements calculating, the annual calcium carbide mud total amount that produces of China reaches about 1,000 ten thousand tons, and traditional main methods is for graving landfill or production cement etc.; Not only need drop into substantial contribution and be used to build environment treating facility, also need take a large amount of soils and be used to deposit waste residue.
Along with China's rapid economy development, Highrise buildings increases, and indoor luxurious decoration strengthens; A large amount of combustiblesubstances gets into various place, and the national wealth and the people's life security in serious threat, only 2007 according to statistics; 15.9 ten thousand of the annual presence of fire altogether of China (not comprising forest, grassland, army, mine underground part fire, down together), dead 1418 people; Injured 863 people, 9.9 hundred million yuan of direct property losss.
Be effective fire containment accident; Protection national wealth and people's life safety; Country constantly puts into effect relevant fire codes and policy; On December 7,2007, the Ministry of Public Security issued " about the notice of further reinforcement public place fire-retardant product management work " specially, and notice is regulation clearly, after 1 day July in 2008; Every use does not meet the fire-retardant product of " public place fire-retardant product and assembly combustionproperty require and sign ", to the fire-fighting of this public place check and accept or opening before the security against fire inspection must not give without exception through.And require fire department when the public place being implemented daily fire supervision inspection; To check the situation of using fire-retardant product; Fire-retardant product is not used in discovery on request, be ordered to make correction within a time limit, and supervises the public place to be replaced by satisfactory fire-retardant product.
Along with the reinforcement of country to public place management of fire safety work, the increase of fire-retardant product consumption, the fire retardant consumption strengthens certainly thereupon; Only be example with sheet material, the annual sheet material total amount of producing of China is about 7000 ten thousand steres, if 10% entering public place uses; Just reach 700 ten thousand steres, with 100 kilograms of fire retardants, only sheet material is one in every cubic metre of need; Need fire retardant just reach 700,000 tons in year, if add solid wood, cotton or the like, the fire retardant demand of China is quite surprising; If adopt other material produce fire retardant, be certain to cause raw material nervous, price is surging; If can utilize calcium carbide waste slag to produce fire retardant, not only found an effective way for the calcium carbide waste slag utilization of China, more can find reliable material guarantee for the mass production of fire retardant.
Summary of the invention
The present invention's technical problem at first to be solved provides a kind of new fire retardant, and this fire retardant mainly is that composition is prepared from the calcium carbide waste slag.
The present invention's technical problem at first to be solved realizes through following technical scheme:
A kind of fire retardant, form by each component of following weight part:
100~400 parts of calcium carbide waste slags, 130~500 parts of thionamic acids, 0~90 part of phosphatase 11,50~200 parts of boric acid; 50~200 parts of boraxs, 0.2~5 part of permeate agent, 1~10 part of polyol; 1~10 part in tensio-active agent, 1~10 part of skimmer, 150~600 parts in 0.2~5 part of santal essence and water.
Preferably, the weight part of each component is: 250 parts of calcium carbide waste slags, 350 parts of thionamic acids, phosphoric acid 60,100 parts of boric acid, 100 parts of boraxs, 2 parts of permeate agents, 5 parts of polyols, 5 parts in tensio-active agent, 5 parts of skimmers, smart 2 parts of santal, 350 parts in water.
Wherein, described thionamic acid can combine with sulfuric acid with urea and replace, wherein, and preferably 100~350 parts of the weight parts of urea, preferably 200~600 parts of vitriolic weight parts.
Described calcium carbide waste slag is to be raw material with the calcium carbide, adds water (wet method) production trade waste that acetylene produced, and is commonly called as carbide slag slurries.
Described permeate agent includes but not limited to: T 46155 ether compound (JFC), sulfated castor oil or succsinic acid alkyl ester sodium sulfonate.
Described polyol is preferably glycerine.
Described tensio-active agent comprises but is not limited to: n-dodecyl mercaptan, terepthaloyl moietie, glycerine tetramethylolmethane, uncle's lauryl mercaptan or sorbyl alcohol.
Described skimmer includes but not limited to: dimethyl silicone oil, Semen Maydis oil or soya-bean oil.
The santal essence is the resulting Lignum Dalbergiae Odoriferae oil in santal (Santalaceae Santalaceae) timber process distillation back, is the fixative of perfume industry.The santal essence can prepare santal timber according to the ordinary method of this area after distilling, also can buy from various commercial sources obtain, for example can be available from the scorching essence and flavoring agent of the gold ltd in the Xiamen.
The used above-mentioned various raw materials of the present invention all can be bought from the chemical industry shop and obtain, and its specification meets industry standard.
Another technical problem to be solved by this invention provides a kind of method for preparing above-mentioned fire retardant.
Another technical problem to be solved by this invention realizes through following technical scheme:
A kind of method for preparing above-mentioned fire retardant comprises:
(1) takes by weighing each component by said weight part;
(2) in reaction kettle, add entry, calcium carbide waste slag, thionamic acid (or urea and sulfuric acid combine surrogate) adds skimmer then; Permeate agent, santal essence and the tensio-active agent that accounts for the 1/2-2/3 of tensio-active agent gross weight are warming up to 110~125 ℃, are incubated 1~3 hour; Be cooled to 65~98 ℃, drip phosphoric acid, be incubated 1~2 hour, be cooled to 60~85 ℃ until being warming up to 110~125 ℃; Add boric acid, borax, polyol; Heat to 100~125 ℃, be incubated 1~3 hour, emit cooling to reaction mass then;
(3) put into the cooling tank that has whipping appts to cooled material, add remaining tensio-active agent, under whipped state, material is cooled to 35~40 ℃, promptly get emulsion fire retardant; Also can be with obtaining solid flame retardant behind the further drying and dewatering of emulsion fire retardant.
The method of use of fire retardant of the present invention: as a reference, can fire retardant of the present invention be mixed with the part by weight of urea-formaldehyde glue according to 1:3-4, stir, have the density board of fire performance again according to the process method production of routine; Perhaps with after the water dilution of fire retardant of the present invention with 8-10 times of weight, press and annotate in the timber, preparation has the timber of fire performance.
Fire retardant of the present invention mainly utilizes calcium carbide waste slag to be prepared from, for the calcium carbide waste residue treatment of China finds one effectively to utilize approach, and prepared fire retardant excellent performance, cheap.Fire retardant of the present invention can be widely used in wood-based plate, timber, cotton, paper etc.
Embodiment
Further describe the present invention below in conjunction with specific embodiment; What those skilled in the art should understand that is; Down can make amendment with form or replace without departing from the spirit and scope of the present invention, but these modifications and replacing all fall in protection scope of the present invention the details of technical scheme of the present invention.
The preparation of embodiment 1 fire retardant
(1) presses the column weight amount and take by weighing each component (unit: kg): calcium carbide waste slag 100, thionamic acid 130, phosphatase 11 0, boric acid 50, borax 50, sulfated castor oil 0.2, glycerine 1, terepthaloyl moietie 1, dimethyl silicone oil 1, santal essence 0.2, water 150;
(2) in reaction kettle, add entry, calcium carbide waste slag, thionamic acid adds dimethyl silicone oil then, the terepthaloyl moietie of 0.5kg; Santal essence and sulfated castor oil are warming up to 110 ℃, are incubated 1~3 hour, are cooled to 65 ℃, drip phosphoric acid to being warming up to 110 ℃; Be incubated 1~2 hour, be cooled to 60 ℃, add boric acid, borax; Glyceryl alcohol is heated to 100 ℃, is incubated 1~3 hour, emits cooling to reaction mass then;
(3) put into the cooling tank that has whipping appts to cooled material, add remaining 0.5kg terepthaloyl moietie, under whipped state, material is cooled to 35 ℃, promptly get emulsion fire retardant; Also can be with obtaining solid flame retardant behind the further drying and dewatering of emulsion fire retardant.
The preparation of embodiment 2 fire retardants
(1) presses the column weight amount and take by weighing each component (unit: kg): calcium carbide waste slag 400, thionamic acid 500, phosphatase 79 0, boric acid 200, borax 200, T 46155 ether compound 5, glycerine 10, sorbyl alcohol 10, dimethyl silicone oil 10, santal essence 5, water 600;
(2) in reaction kettle, add entry, calcium carbide waste slag, thionamic acid adds dimethyl silicone oil then, the sorbyl alcohol of 6.7kg; Smart and the T 46155 ether compound of santal is warming up to 125 ℃, is incubated 1~3 hour, is cooled to 98 ℃, drips phosphoric acid and is warming up to 125 ℃ automatically by it; Be incubated 1~2 hour, be cooled to 85 ℃, add boric acid, borax; Glycerine is heated to 1255 ℃, is incubated 1~3 hour, emits cooling to reaction mass then;
(3) put into the cooling tank that has whipping appts to cooled material, add the sorbyl alcohol of remaining 3.3kg, under whipped state, material is cooled to 40 ℃, promptly get emulsion fire retardant; Also can be with obtaining solid flame retardant behind the further drying and dewatering of emulsion fire retardant.
The preparation of embodiment 3 fire retardants
(1) presses the column weight amount and take by weighing each component (unit: kg): calcium carbide waste slag 250, thionamic acid 350, phosphoric acid 60, boric acid 100, borax 100, T 46155 ether compound 2, glycerine 5, n-dodecyl mercaptan 5, dimethyl silicone oil 5, santal essence 2, water 350;
(2) in reaction kettle, add entry, calcium carbide waste slag, thionamic acid adds dimethyl silicone oil then, the n-dodecyl mercaptan of 2.5kg; Smart and the T 46155 ether compound of santal is warming up to 120 ℃, is incubated 1~3 hour, is cooled to 85 ℃, drips phosphoric acid until being warming up to 115 ℃; Be incubated 1~2 hour, be cooled to 75 ℃, add boric acid, borax; The polyol glyceryl alcohol is heated to 850 ℃, is incubated 1~3 hour, emits cooling to reaction mass then;
(3) put into the cooling tank that has whipping appts to cooled material, add the n-dodecyl mercaptan of residue 2.5kg, under whipped state, material is cooled to 38 ℃, promptly get emulsion fire retardant; Also can be with obtaining solid flame retardant behind the further drying and dewatering of emulsion fire retardant.
The preparation of embodiment 4 fire retardants
(1) presses the column weight amount and take by weighing each component (unit: kg): calcium carbide waste slag 100, urea 100, sulfuric acid 200, phosphatase 11 0, boric acid 50, borax 50, succsinic acid alkyl fat sodium sulfonate 0.2, glycerine 1, n-dodecyl mercaptan 1, dimethyl silicone oil 1, santal essence 0.2, water 150;
(2) in reaction kettle, add entry, calcium carbide waste slag, urea, sulfuric acid adds dimethyl silicone oil then; 0.67kg n-dodecyl mercaptan, the smart and succsinic acid alkyl ester sodium sulfonate of santal is warming up to 110 ℃, is incubated 1~3 hour, is cooled to 65 ℃; Drip phosphoric acid until being warming up to 110 ℃, be incubated 1~2 hour, be cooled to 60 ℃, add boric acid, borax; Glyceryl alcohol is heated to 500 ℃, is incubated 1~3 hour, emits cooling to reaction mass then;
(3) put into the cooling tank that has whipping appts to cooled material, add the n-dodecyl mercaptan of remaining 0.33kg, under whipped state, material is cooled to 40 ℃, promptly get emulsion fire retardant; Also can be with obtaining solid flame retardant behind the further drying and dewatering of emulsion fire retardant.
The preparation of embodiment 5 fire retardants
(1) presses the column weight amount and take by weighing each component (unit: kg): calcium carbide waste slag 400, urea 350, sulfuric acid 600, phosphoric acid 50, boric acid 200, borax 200, T 46155 ether compound 5, glycerine 10, uncle's lauryl mercaptan 10, Semen Maydis oil 10, santal essence 5, water 600;
(2) in reaction kettle, add entry, calcium carbide waste slag, urea, sulfuric acid adds Semen Maydis oil then; Uncle's lauryl mercaptan of 5kg, the smart and T 46155 ether compound of santal is warming up to 120 ℃, is incubated 1~3 hour, is cooled to 90 ℃; Drip phosphoric acid, let it be warming up to 115 ℃ automatically, be incubated 1~2 hour, be cooled to 75 ℃, add boric acid; Borax, glycerine is heated to 1000 ℃, is incubated 1~3 hour, emits cooling to reaction mass then;
(3) put into the cooling tank that has whipping appts to cooled material, add remaining uncle's 5kg lauryl mercaptan, under whipped state, material is cooled to 40 ℃, promptly get emulsion fire retardant; Also can be with obtaining solid flame retardant behind the further drying and dewatering of emulsion fire retardant.
The flame retardant properties test of Test Example 1 fire retardant of the present invention
70 kilograms of the fire retardants that embodiment 1 is prepared; Add in the urea-formaldehyde glue of 220-250 kilogram; Stir; The production density plate, through detecting (detect according to national standard " public place fire-retardant product and assembly combustionproperty require and sign " method (GB20086-2006) and carry out), the fire resistance rating of institute's production density plate reaches the C level of national standard.
The fire retardant 120 kg that embodiment 2 is prepared; Add in the urea-formaldehyde glue of 220-250 kilogram; Stir; The production density plate, through detecting (detect according to national standard " public place fire-retardant product and assembly combustionproperty require and sign " method (GB20086-2006) and carry out), the fire resistance rating of institute's production density plate reaches national standard B level.
160 kilograms of the fire retardants that embodiment 3 is prepared; Add in the urea-formaldehyde glue of 220-250 kilogram; Stir; The production density plate, through detecting (detect according to national standard " public place fire-retardant product and assembly combustionproperty require and sign " method (GB20086-2006) and carry out), the fire resistance rating of institute's production density plate reaches the A of national standard
2Level.
The fire retardant 120 kg that embodiment 4 is prepared; Add in the urea-formaldehyde glue of 220-250 kilogram; Stir; The production density plate, through detecting (detect according to national standard " public place fire-retardant product and assembly combustionproperty require and sign " method (GB20086-2006) and carry out), the fire resistance rating of institute's production density plate reaches the B level of national standard.
The fire retardant 120 kg that embodiment 5 is prepared; Add in the urea-formaldehyde glue of 220-250 kilogram; Stir; The production density plate, through detecting (detect according to national standard " public place fire-retardant product and assembly combustionproperty require and sign " method (GB20086-2006) and carry out), the fire resistance rating of institute's production density plate reaches the B level of national standard.
The flame retardant properties test of Test Example 2 fire retardants of the present invention
80 kilograms of the fire retardants that embodiment 1 is prepared; Dilute with 600 kg of water; Pressure is annotated in the timber; Through detecting (detect according to national standard " public place fire-retardant product and assembly combustionproperty require and sign " method (GB20086-2006) and carry out), the fire resistance rating of the timber of annotating of pressing reaches the C level of national standard.
80 kilograms of the fire retardants that embodiment 2 is prepared; Dilute with 600 kg of water; Pressure is annotated timber; Through detecting (detect according to national standard " public place fire-retardant product and assembly combustionproperty require and sign " method (GB20086-2006) and carry out), the fire resistance rating of the timber of annotating of pressing reaches the C level of national standard.
100 kilograms of the fire retardants that embodiment 3 is prepared; Dilute with 800 kg of water; Pressure is annotated timber; Through detecting (detect according to national standard " public place fire-retardant product and assembly combustionproperty require and sign " method (GB20086-2006) and carry out), the fire resistance rating of the timber of annotating of pressing reaches the B level of national standard.
The fire retardant 120 kg that embodiment 4 is prepared; Dilute with 1000 kg of water; Pressure is annotated timber; Through detecting (detect according to national standard " public place fire-retardant product and assembly combustionproperty require and sign " method (GB20086-2006) and carry out), the fire resistance rating of the timber of annotating of pressing reaches the B level of national standard.
100 kilograms of the fire retardants that embodiment 5 is prepared; Dilute with 800 kg of water; Pressure is annotated timber; Through detecting (detect according to national standard " public place fire-retardant product and assembly combustionproperty require and sign " method (GB20086-2006) and carry out), the fire resistance rating of the timber of annotating of pressing reaches the C level of national standard.
Claims (6)
1. a fire retardant is made up of each component of following weight part: 100~400 parts of calcium carbide waste slags, 130~500 parts of thionamic acids; 0~90 part of phosphatase 11,50~200 parts of boric acid, 50~200 parts of boraxs; 0.2~5 part of permeate agent, 1~10 part of polyol, 1~10 part in tensio-active agent; 1~10 part of skimmer, 150~600 parts in 0.2~5 part of santal essence and water, described permeate agent is selected from T 46155 ether compound, sulfated castor oil or succsinic acid alkyl ester sodium sulfonate; Said polyol is a glycerine; Described tensio-active agent is selected from n-dodecyl mercaptan, terepthaloyl moietie, glycerine, tetramethylolmethane, uncle's lauryl mercaptan or sorbyl alcohol, and described skimmer is selected from dimethyl silicone oil, Semen Maydis oil or soya-bean oil.
2. according to the described fire retardant of claim 1, it is characterized in that the weight part of each component is: 250 parts of calcium carbide waste slags, 350 parts of thionamic acids; 60 parts of phosphoric acid, 100 parts of boric acid, 100 parts of boraxs; 2 parts of permeate agents, 5 parts of polyols, 5 parts in tensio-active agent; 5 parts of skimmers, smart 2 parts of santal, 350 parts in water.
3. according to the described fire retardant of claim 1, it is characterized in that: said thionamic acid is combined by urea and sulfuric acid and replaces; Wherein, the weight part of urea is 100~350 parts, and the vitriolic weight part is 200~600 parts.
4. method for preparing claim 1 or 2 said fire retardants comprises:
(1) takes by weighing each component by claim 1 or 2 said weight part proportionings;
(2) in reaction kettle, add entry, calcium carbide waste slag, thionamic acid or urea and sulfuric acid add skimmer then; Permeate agent, santal essence and the tensio-active agent that accounts for tensio-active agent gross weight 1/2-2/3 are warming up to 110~125 ℃, are incubated 1~3 hour; Be cooled to 65~98 ℃, drip phosphoric acid, be incubated 1~2 hour, be cooled to 60~85 ℃ until being warming up to 110~125 ℃; Add boric acid, borax, polyol; Heat to 100~125 ℃, be incubated 1~3 hour, emit cooling to reaction mass then;
(3) put into the cooling tank that has whipping appts to cooled material, add remaining tensio-active agent, under whipped state, material is cooled to 35~40 ℃, promptly get emulsion fire retardant.
5. according to the described preparation method of claim 4, it is characterized in that: the further drying and dewatering of emulsion fire retardant is obtained solid flame retardant.
6. artificial board, timber, cotton or paper that preparation has fire performance are used it in the application of claim 1 or 2 described fire retardants.
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CN101724413B true CN101724413B (en) | 2012-03-21 |
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CN109972417A (en) * | 2019-04-04 | 2019-07-05 | 六安市海洋羽毛有限公司 | A kind of preparation process of fire-retardant fluffy plumage weaving material |
CN116787566B (en) * | 2023-07-24 | 2024-03-08 | 南京林业大学 | Sulfonated straw flame retardant, and preparation method and application thereof |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1249325A (en) * | 1998-09-28 | 2000-04-05 | 于宝立 | Flame-retarding agent |
CN1331267A (en) * | 2000-06-26 | 2002-01-16 | 淄博市临淄镭射技术研究所 | Natural water-base fire-retarding adhesive |
CN1911613A (en) * | 2006-08-23 | 2007-02-14 | 李佐明 | Wood fire retardant and wood fire retarding treatment technology |
-
2008
- 2008-10-17 CN CN2008101679194A patent/CN101724413B/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1249325A (en) * | 1998-09-28 | 2000-04-05 | 于宝立 | Flame-retarding agent |
CN1331267A (en) * | 2000-06-26 | 2002-01-16 | 淄博市临淄镭射技术研究所 | Natural water-base fire-retarding adhesive |
CN1911613A (en) * | 2006-08-23 | 2007-02-14 | 李佐明 | Wood fire retardant and wood fire retarding treatment technology |
Non-Patent Citations (1)
Title |
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JP特开2003-246986A 2003.09.05 |
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