CN104909388A - Research of information automation production technology for combined production of cyanuric acid and ammonium sulfate, and synthesis and research of chloro derivative - Google Patents
Research of information automation production technology for combined production of cyanuric acid and ammonium sulfate, and synthesis and research of chloro derivative Download PDFInfo
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- CN104909388A CN104909388A CN201510238729.7A CN201510238729A CN104909388A CN 104909388 A CN104909388 A CN 104909388A CN 201510238729 A CN201510238729 A CN 201510238729A CN 104909388 A CN104909388 A CN 104909388A
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Abstract
The invention especially relates to research of an information automation production technology for combined production of cyanuric acid and ammonium sulfate, and synthesis and research of a chloro derivative. The information automation production technology for combined production of cyanuric acid and ammonium sulfate comprises the following steps: adding urea, hydrogen peroxide and water into a reaction container according to a molar ratio of urea to hydrogen peroxide of 1:0.3, adding zinc nitrate and copper nitrate, heating, adding cold water, repeating, drying to obtain cyanuric acid, allowing waste gas to enter a saturator, and adding sulfuric acid to generate an ammonium sulfate solution; and sending the ammonium sulfate solution to a crystallization kettle, cooling for crystallizing, and drying ammonium sulfate crystals. The cyanuric acid preparation technology increases the yield to 92.5% from original yield, generated waste gas can be directly used for producing ammonium sulfate to avoid environment pollution and resource waste, and a control system is arranged to make the further reinforcement of the safety coefficient of the working environment convenient.
Description
(1) technical field
The present invention relates to cyanuric acid, particularly a kind of research of cyanuric acid coproduction of ammonia sulfate information automation production technique and the synthesis of chlorinated derivative and research.
(2) background technology
Cyanuric acid (CA) belongs to the intermediate of Organic Chemicals, apply extremely extensive, be mainly used in cyanuric acid chloride, salt, the producing of ester class, the synthesis of SYNTHETIC OPTICAL WHITNER, resin, oxidation inhibitor, paint, selective herbicide and metal cyanide negative catalyst, and as the additive of nylon, fire-retardant for plastic and makeup, occupy an important position in organic synthesis.CN1121513A discloses a kind of cyanuric acid prepared by solvent induced pyrolysis method, it be urea in a certain amount of hydrogen peroxide and a small amount of water, with platinic compound or copper compound or platinum, copper compound for catalyzer, household microwave oven or electric furnace heat, make its rapid reaction, obtain cyanuric acid.Again cyanuric acid is dissolved in hot water, allows its cooling leave standstill, the cyanuric acid of 2 crystal water can be contained.This method can complete reaction in 2-10 minute.Its yield can reach more than 80%, and without the three wastes, described waste gas is ammonia, and direct discharge can cause the pollution of environment, and direct discharge then can cause serious environmental pollution, and is a kind of waste of resource.But its yield still needs to improve.
Trichloroisocyanuric acid, organic compound, white crystalline powder or granular solids, have strong chlorine pungent taste.Trichloroisocyanuric acid is a kind of extremely strong oxygenant and chlorizating agent, has efficient, wide spectrum, safer disinfection, has killing action, also have certain killing effect to coccidian oocyst to bacterium, virus, fungi, gemma etc.Trichloroisocyanuric acid is one of chlorated fulminuric acid series product, the chloro-s-triazine 2 of formal name used at school three, 4,6(1H, 3H, 5H) triketone, English name Trichl0ID-isocyantlric Acid. is called for short TCCA, and sterling is powdery white crystallization, available chlorine theoretical content 91.54%, industrial goods available chlorine content is not less than 85%, and active chlorine content is higher than chlorinated lime 2 ~ 3 times.Trichloroisocyanuric acid is the renewal product of chlorinated lime, calcium hypochlorite, and the three wastes reduce greatly than calcium hypochlorite, the trend of advanced country's its alternative calcium hypochlorite useful.
But because CA chlorination is prepared in TCCA process, containing more by-product allophanamide, carbonyldiurea, melon and unreacted raw material urea in CA, NCl3 is generated with chlorine reaction, CA easily generates NCl3 in basic solution, TCCA product is being heated or also can decomposing generation NCl3 under alkaline condition, and introduce chlorine gas to make reaction carries out in encloses container, as everyone knows, NCl3, accumulation is very easily blasted.
For improving the security of chloridization process, the stability of strengthen operation, various countries research worker has done a large amount of research work, patent disclosed in December 1 in 2010: utilize calcium carbonate to produce the technique of trichloroisocyanuric acid, this technique: first chlorine and water generation hydrolysis reaction, then hydrolysate and calcium carbonate and cyanuric acid react respectively and generate side product chlorinated calcium and trichloroisocyanuric acid, owing to not using the strong alkaline substances such as sodium hydroxide in whole reaction, reaction system is in neutral or weakly alkaline, doing so avoids chlorine and cyanuric acid broken ring derivatives occurs to react the risk generating nitrogen trichloride, the security of production technique improves greatly, and the calcium carbonate cost used in this technique comparatively alkali lye significantly reduce, and the particle diameter of calcium carbonate is also had no requirement, so the cost of technique of the present invention significantly reduces.But fast and safely generate, be still the target that we pursue.
(3) summary of the invention
The present invention, in order to make up the deficiencies in the prior art, provides a kind of protection of the environment, reduces costs, the research of cyanuric acid coproduction of ammonia sulfate information automation production technique of operational safety and the synthesis of chlorinated derivative and research.
The present invention is achieved through the following technical solutions:
A kind of cyanuric acid coproduction of ammonia sulfate information automation production technique, its special character is: comprise the following steps:
(1) in reaction vessel, urea, hydrogen peroxide and water is added, wherein, the mol ratio of urea and hydrogen peroxide is 1:0.3, then adds zinc nitrate and cupric nitrate, heating, repeatedly repeat through cold water again, obtain cyanuric acid after oven dry, zinc nitrate consumption is the 2-4% of weight of urea, and cupric nitrate consumption is 2% of weight of urea, the waste gas that reaction vessel produces enters the saturex for generating ammonium sulfate, adds sulfuric acid and generate ammoniumsulphate soln in saturex;
(2) ammoniumsulphate soln is sent to crystallization kettle crystallisation by cooling, isolates ammonia sulfate crystal through whizzer;
(3) ammonia sulfate crystal is placed in baker, dries ammonia sulfate crystal.
Cyanuric acid coproduction of ammonia sulfate information automation production technique of the present invention, in the solution that hydrogen peroxide and water are formed, concentration of hydrogen peroxide is 27.5%.
Cyanuric acid coproduction of ammonia sulfate information automation production technique of the present invention, also adds sulphuric acid soln, and the mol ratio of urea and sulfuric acid is 1:0.1.
Cyanuric acid coproduction of ammonia sulfate information automation production technique of the present invention, reaction vessel, saturex, crystallization kettle, whizzer, baker are all connected with Controlling System, described Controlling System comprises C8051F020,39VF080, DM13A chip, power up function device of swiping the card comprises card reader ZD2D01, relay J W1FSN-DC12V, silicon controlled rectifier BT169, and automatic dialing warning device comprises STC12C5410 and MT8888 chip.
A method for the cyanuric acid synthesis chlorinated derivative of preparation, its special character is: the preparation of trichloroisocyanuric acid comprises the following steps:
In a kettle., add calcium carbonate, water, at room temperature first lead to chlorine, and then add calcium hydroxide aqueous solution, described calcium hydroxide aqueous solution directly adds to below liquid level, extract hypochlorous acid again, react with cyanuric acid solution, obtain trichloroisocyanuric acid after filtering drying, wherein, the mol ratio of cyanuric acid and calcium carbonate and calcium hydroxide is 1:1.6, and the mol ratio of calcium carbonate and calcium hydroxide is 8:2-3.
The method of synthesis chlorinated derivative of the present invention, the preparation of DICHLOROISOCYANURIC ACID comprises the following steps:
Cyanuric acid, calcium carbonate, calcium hydroxide and water are placed in batching kettle by weight 1: 0.5:0.4: 8 and are mixed with cyanuric acid calcium solution, the cyanuric acid calcium solution prepared is sent in absorption tower, the chlorine residue waste gas produced in trichloroisocyanuric acid reaction process is introduced absorption tower absorb, control absorption tower temperature at 29 DEG C, be terminal when cyanuric acid calcium liquid absorbs chlorine residue to pH value 1.7-2.5, in absorption tower, material is put into crystallization kettle and is carried out crystallization, through centrifuge dehydration, dries to obtain dichloro isocyanuric urine acid product.
Beneficial effect of the present invention: the present invention prepares the technique of cyanuric acid on original basis, further increase yield, yield can reach 92.5%, the waste gas produced is directly used in production ammonium sulfate, avoid the waste of environmental pollution and resource, the safety coefficient strengthening Working environment is further convenient in the setting of Controlling System, calcium carbonate replaces sodium hydroxide and produces in trichloroisocyanuric acid process, solution is in neutral, so ring can not be there is brokenly in cyanuric acid, also nitrogen trichloride can not be generated with chlorine after passing into chlorine, this also just avoids the danger generating by product nitrogen trichloride and blast, process safety improves greatly, be worthy to be popularized, and pass through the interpolation of the calcium hydroxide aqueous solution aqueous solution, accelerate chlorine and generate hypochlorous acid, and calcium hydroxide continues to produce hypochlorous acid by the calcium carbonate that reaction produces.Simple to operate, action condition is gentle, easily grasp, with short production cycle.
(4) embodiment
Embodiment 1
The present embodiment cyanuric acid coproduction of ammonia sulfate information automation production technique, comprises the following steps:
(1) in reaction vessel, urea, hydrogen peroxide and water is added, wherein, the mol ratio of urea and hydrogen peroxide is 1:0.3, adds water and makes concentration of hydrogen peroxide be 27.5%, then zinc nitrate and cupric nitrate is added, heating, more repeatedly repeat through cold water, obtain cyanuric acid after oven dry, zinc nitrate consumption is 2% of weight of urea, cupric nitrate consumption is 2% of weight of urea, and the waste gas that reaction vessel produces enters the saturex for generating ammonium sulfate, adds sulfuric acid and generate ammoniumsulphate soln in saturex;
(2) ammoniumsulphate soln is sent to crystallization kettle crystallisation by cooling, isolates ammonia sulfate crystal through whizzer;
(3) ammonia sulfate crystal is placed in baker, dries ammonia sulfate crystal.
Reaction vessel, saturex, crystallization kettle, whizzer, baker is all connected with Controlling System, and this Controlling System comprises C8051F020, 39VF080, DM13A chip, Controlling System can also connect fingerprint identification device or/and power up function device of swiping the card, and wherein fingerprint identification device is by P-80 fingerprint machine, relay J W1FSN-DC12V, the compositions such as silicon controlled rectifier BT169, power up function device of swiping the card is by card reader ZD2D01, relay J W1FSN-DC12V, the compositions such as silicon controlled rectifier BT169, fingerprint identification device, swiping the card power up function device can standard operation people, avoid misoperation, automatic dialing warning device, comprise STC12C5410 and MT8888, user can prestore the alarm call number of person skilled in micro-chip storer by keyboard, after having guard signal to send micro-chip to, micro-chip is by the right of priority according to alert, dial corresponding telephone number and provide voice message, the telephone network of the long-distance intelligent telephone automatic alarming system consisted of STC12C5410 and MT8888 sends to user.Automatic dialing warning device also can comprise micro-chip, the receiver module be connected with micro-chip respectively, alarm center, GSM module, wherein GSM module is connected with landline telephone, mobile phone wireless, and receiver module is connected with treatment system and the warning signal received is passed to micro-chip and processes.When reaction vessel, saturex, crystallization kettle, whizzer, baker have a problem, can staff be notified, Timeliness coverage problem, guarantee the safety of production process.
The preparation of trichloroisocyanuric acid comprises the following steps:
In a kettle., calcium carbonate 14kg, 260kg water, at room temperature first lead to chlorine, then add 0.0115mol/L calcium hydroxide aqueous solution, described calcium hydroxide aqueous solution directly adds to below liquid level, and the mol ratio of calcium carbonate and calcium hydroxide is 8:2, react under agitation, during pH value 4.6, add the cyanuric acid aqueous solution (30%) and react, wherein cyanuric acid content is 12.9kg, trichloroisocyanuric acid 23kg is obtained, effective cyanogen 92.1% after filtering drying.
The preparation of DICHLOROISOCYANURIC ACID comprises the following steps:
Cyanuric acid, calcium carbonate, calcium hydroxide and water are placed in batching kettle by weight 1: 0.5:0.4: 8 and are mixed with cyanuric acid calcium solution, the cyanuric acid calcium solution prepared is sent in absorption tower, the chlorine residue waste gas produced in trichloroisocyanuric acid reaction process is introduced absorption tower absorb, control absorption tower temperature at 29 DEG C, be terminal when cyanuric acid calcium liquid absorbs chlorine residue to pH value 1.7-2.5, in absorption tower, material is put into crystallization kettle and is carried out crystallization, through centrifuge dehydration, dries to obtain dichloro isocyanuric urine acid product.
Embodiment 2
The present embodiment cyanuric acid coproduction of ammonia sulfate information automation production technique, comprises the following steps:
(1) in reaction vessel, urea, hydrogen peroxide and water is added, wherein, the mol ratio of urea and hydrogen peroxide is 1:0.3, adds water and makes concentration of hydrogen peroxide be 27.5%, then zinc nitrate and cupric nitrate is added, heating, more repeatedly repeat through cold water, obtain cyanuric acid after oven dry, zinc nitrate consumption is 3% of weight of urea, cupric nitrate consumption is 2% of weight of urea, and the waste gas that reaction vessel produces enters the saturex for generating ammonium sulfate, adds sulfuric acid and generate ammoniumsulphate soln in saturex;
(2) ammoniumsulphate soln is sent to crystallization kettle crystallisation by cooling, isolates ammonia sulfate crystal through whizzer;
(3) ammonia sulfate crystal is placed in baker, dries ammonia sulfate crystal.
Reaction vessel, saturex, crystallization kettle, whizzer, baker is all connected with Controlling System, and this Controlling System comprises C8051F020, 39VF080, DM13A chip, Controlling System can also connect fingerprint identification device or/and power up function device of swiping the card, and wherein fingerprint identification device is by P-80 fingerprint machine, relay J W1FSN-DC12V, the compositions such as silicon controlled rectifier BT169, power up function device of swiping the card is by card reader ZD2D01, relay J W1FSN-DC12V, the compositions such as silicon controlled rectifier BT169, fingerprint identification device, swiping the card power up function device can standard operation people, avoid misoperation, automatic dialing warning device, comprise STC12C5410 and MT8888, user can prestore the alarm call number of person skilled in micro-chip storer by keyboard, after having guard signal to send micro-chip to, micro-chip is by the right of priority according to alert, dial corresponding telephone number and provide voice message, the telephone network of the long-distance intelligent telephone automatic alarming system consisted of STC12C5410 and MT8888 sends to user.Automatic dialing warning device also can comprise micro-chip, the receiver module be connected with micro-chip respectively, alarm center, GSM module, wherein GSM module is connected with landline telephone, mobile phone wireless, and receiver module is connected with treatment system and the warning signal received is passed to micro-chip and processes.When reaction vessel, saturex, crystallization kettle, whizzer, baker have a problem, can staff be notified, Timeliness coverage problem, guarantee the safety of production process.
The preparation of trichloroisocyanuric acid comprises the following steps:
In a kettle., calcium carbonate 14kg, 260kg water, at room temperature first lead to chlorine, then add 0.0115mol/L calcium hydroxide aqueous solution, described calcium hydroxide aqueous solution directly adds to below liquid level, and the mol ratio of calcium carbonate and calcium hydroxide is 8:3, react under agitation, during pH value 4.6, add the cyanuric acid aqueous solution (30%) and react, wherein cyanuric acid content is 12.9kg, trichloroisocyanuric acid 22.9kg is obtained, effective cyanogen 92.4% after filtering drying.
The preparation of DICHLOROISOCYANURIC ACID comprises the following steps:
Cyanuric acid, calcium carbonate, calcium hydroxide and water are placed in batching kettle by weight 1: 0.5:0.4: 8 and are mixed with cyanuric acid calcium solution, the cyanuric acid calcium solution prepared is sent in absorption tower, the chlorine residue waste gas produced in trichloroisocyanuric acid reaction process is introduced absorption tower absorb, control absorption tower temperature at 29 DEG C, be terminal when cyanuric acid calcium liquid absorbs chlorine residue to pH value 1.7-2.5, in absorption tower, material is put into crystallization kettle and is carried out crystallization, through centrifuge dehydration, dries to obtain dichloro isocyanuric urine acid product.
Embodiment 3
The present embodiment cyanuric acid coproduction of ammonia sulfate information automation production technique, comprises the following steps:
(1) in reaction vessel, urea is added, hydrogen peroxide, sulphuric acid soln (55%) and water, wherein, the mol ratio of urea and sulfuric acid is 1:0.1, the mol ratio of urea and hydrogen peroxide is 1:0.3, add water and make concentration of hydrogen peroxide be 27.5%, then zinc nitrate and cupric nitrate is added, heating, repeatedly repeat through cold water again, cyanuric acid (yield is up to 93.4%) is obtained after oven dry, zinc nitrate consumption is 4% of weight of urea, cupric nitrate consumption is 2% of weight of urea, the waste gas that reaction vessel produces enters the saturex for generating ammonium sulfate, add sulfuric acid in saturex and generate ammoniumsulphate soln,
(2) ammoniumsulphate soln is sent to crystallization kettle crystallisation by cooling, isolates ammonia sulfate crystal through whizzer;
(3) ammonia sulfate crystal is placed in baker, dries ammonia sulfate crystal.
Cyanuric acid coproduction of ammonia sulfate information automation production technique of the present invention, in the solution that hydrogen peroxide and water are formed.
Reaction vessel, saturex, crystallization kettle, whizzer, baker is all connected with Controlling System, and this Controlling System comprises C8051F020, 39VF080, DM13A chip, Controlling System can also connect fingerprint identification device or/and power up function device of swiping the card, and wherein fingerprint identification device is by P-80 fingerprint machine, relay J W1FSN-DC12V, the compositions such as silicon controlled rectifier BT169, power up function device of swiping the card is by card reader ZD2D01, relay J W1FSN-DC12V, the compositions such as silicon controlled rectifier BT169, fingerprint identification device, swiping the card power up function device can standard operation people, avoid misoperation, automatic dialing warning device, comprise STC12C5410 and MT8888, user can prestore the alarm call number of person skilled in micro-chip storer by keyboard, after having guard signal to send micro-chip to, micro-chip is by the right of priority according to alert, dial corresponding telephone number and provide voice message, the telephone network of the long-distance intelligent telephone automatic alarming system consisted of STC12C5410 and MT8888 sends to user.Automatic dialing warning device also can comprise micro-chip, the receiver module be connected with micro-chip respectively, alarm center, GSM module, wherein GSM module is connected with landline telephone, mobile phone wireless, and receiver module is connected with treatment system and the warning signal received is passed to micro-chip and processes.When reaction vessel, saturex, crystallization kettle, whizzer, baker have a problem, can staff be notified, Timeliness coverage problem, guarantee the safety of production process.
The preparation of trichloroisocyanuric acid comprises the following steps:
In a kettle., add calcium carbonate, water, at room temperature first lead to chlorine, and then add calcium hydroxide aqueous solution, described calcium hydroxide aqueous solution directly adds to below liquid level, extract hypochlorous acid again, react with cyanuric acid solution, obtain trichloroisocyanuric acid after filtering drying, wherein, the mol ratio of cyanuric acid and calcium carbonate and calcium hydroxide is 1:1.6, and the mol ratio of calcium carbonate and calcium hydroxide is 8:2-3.
The preparation of DICHLOROISOCYANURIC ACID comprises the following steps:
Cyanuric acid, calcium carbonate, calcium hydroxide and water are placed in batching kettle by weight 1: 0.5:0.4: 8 and are mixed with cyanuric acid calcium solution, the cyanuric acid calcium solution prepared is sent in absorption tower, the chlorine residue waste gas produced in trichloroisocyanuric acid reaction process is introduced absorption tower absorb, control absorption tower temperature at 29 DEG C, be terminal when cyanuric acid calcium liquid absorbs chlorine residue to pH value 1.7-2.5, in absorption tower, material is put into crystallization kettle and is carried out crystallization, through centrifuge dehydration, dries to obtain dichloro isocyanuric urine acid product.
Claims (6)
1. a cyanuric acid coproduction of ammonia sulfate information automation production technique, its feature part is: comprise the following steps:
(1) in reaction vessel, urea, hydrogen peroxide and water is added, wherein, the mol ratio of urea and hydrogen peroxide is 1:0.3, then adds zinc nitrate and cupric nitrate, heating, repeatedly repeat through cold water again, obtain cyanuric acid after oven dry, zinc nitrate consumption is the 2-4% of weight of urea, and cupric nitrate consumption is 2% of weight of urea, the waste gas that reaction vessel produces enters the saturex for generating ammonium sulfate, adds sulfuric acid and generate ammoniumsulphate soln in saturex;
(2) ammoniumsulphate soln is sent to crystallization kettle crystallisation by cooling, isolates ammonia sulfate crystal through whizzer;
(3) ammonia sulfate crystal is placed in baker, dries ammonia sulfate crystal.
2. cyanuric acid coproduction of ammonia sulfate information automation production technique according to claim 1, its feature part is: in the solution that hydrogen peroxide and water are formed, concentration of hydrogen peroxide is 27.5%.
3. cyanuric acid coproduction of ammonia sulfate information automation production technique according to claim 2, its feature part is: also add sulphuric acid soln, and the mol ratio of urea and sulfuric acid is 1:0.1.
4. cyanuric acid coproduction of ammonia sulfate information automation production technique according to claim 1, its feature part is: reaction vessel, saturex, crystallization kettle, whizzer, baker are all connected with Controlling System, described Controlling System comprises C8051F020,39VF080, DM13A chip, power up function device of swiping the card comprises card reader ZD2D01, relay J W1FSN-DC12V, silicon controlled rectifier BT169, and automatic dialing warning device comprises STC12C5410 and MT8888 chip.
5. synthesize a method for chlorinated derivative with cyanuric acid prepared by claim 1, its feature part is: the preparation of trichloroisocyanuric acid comprises the following steps:
In a kettle., add calcium carbonate, water, at room temperature first lead to chlorine, and then add calcium hydroxide aqueous solution, described calcium hydroxide aqueous solution directly adds to below liquid level, extract hypochlorous acid again, react with cyanuric acid solution, obtain trichloroisocyanuric acid after filtering drying, wherein, the mol ratio of cyanuric acid and calcium carbonate and calcium hydroxide is 1:1.6, and the mol ratio of calcium carbonate and calcium hydroxide is 8:2-3.
6. the method for synthesis chlorinated derivative according to claim 4, its feature part is: the preparation of DICHLOROISOCYANURIC ACID comprises the following steps:
Cyanuric acid, calcium carbonate, calcium hydroxide and water are placed in batching kettle by weight 1: 0.5:0.4: 8 and are mixed with cyanuric acid calcium solution, the cyanuric acid calcium solution prepared is sent in absorption tower, the chlorine residue waste gas produced in trichloroisocyanuric acid reaction process is introduced absorption tower absorb, control absorption tower temperature at 29 DEG C, be terminal when cyanuric acid calcium liquid absorbs chlorine residue to pH value 1.7-2.5, in absorption tower, material is put into crystallization kettle and is carried out crystallization, through centrifuge dehydration, dries to obtain dichloro isocyanuric urine acid product.
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Cited By (1)
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| CN109809433A (en) * | 2019-03-27 | 2019-05-28 | 重庆万盛川东化工有限公司 | Cyanic acid process for producing sodium |
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Application publication date: 20150916 |