CN103396678A - Process for preparing heavy nitrogen solution of permanent yellow G - Google Patents
Process for preparing heavy nitrogen solution of permanent yellow G Download PDFInfo
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- CN103396678A CN103396678A CN2013103295467A CN201310329546A CN103396678A CN 103396678 A CN103396678 A CN 103396678A CN 2013103295467 A CN2013103295467 A CN 2013103295467A CN 201310329546 A CN201310329546 A CN 201310329546A CN 103396678 A CN103396678 A CN 103396678A
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- diazo liquid
- permanent yellow
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- sodium nitrite
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Abstract
The invention discloses a process for preparing a heavy nitrogen solution of permanent yellow G. The process comprises the following steps of: (1) dichlorine pulping, namely adding 1,450-1,550 KG of water, 265-295 KG of 27-34% hydrochloric acid and 170-190 KG of dichlorine into a diazotization barrel, stirring, adding a de-foaming agent, pulping for at least one hour and cooling to the temperature of below zero DEG C; (2) diazotization, namely quickly adding 100-105 KG of 32-42% sodium nitrite into the diazotization barrel within 2 minutes, stirring, preserving the heat to be less than 5 DEG C, adding 8-12 KG of aid, stirring for 3-10 minutes at the temperature of less than 5 DEG C, adding water to ensure that the total volume of the diazotization barrel reaches 2,700-2,850 L, and adding sulfamic acid to remove the redundant sodium nitrite; (3) stopping stirring, and performing suction filtration. According to the process, redundant dichlorine is avoided in proportioning of the dichlorine and the hydrochloric acid, so that self-coupling reaction of the dichlorine can be avoided; the temperature of the solution is reduced to below zero DEG C, so that little toxic gas is produced.
Description
Technical field
The present invention relates to a kind of sub-complete processing of coating, be specifically related to the preparation technology of the diazo liquid of a kind of permanent yellow G.
Background technology
Along with growth in the living standard, pigment, coating are widely used in people's life, can be used for the living environment of beautifying people.For better coating, the place of pigment is used in order to reach high-resolution requirement in many places, needs the production regular shape, the pigment of good fluidity.At present, existing pigment be all generally through mixing, the technique preparations such as mixing, pulverizing, classification, outer doping.The preparation of pigment generally comprises and first prepares diazo liquid, then make pigment with other additive reactions, control parameter in existing diazo liquid manufacture craft technique arranges undesirable, the reaction that easily produces the two chlorine of raw material and Sodium Nitrite obtains toxic gas nitrogen protoxide and nitrogen peroxide etc., can work the mischief to people.
Summary of the invention
The object of the invention is to:, for the deficiencies in the prior art, the invention provides a kind of.
The preparation technology of the diazo liquid of a kind of permanent yellow G comprises the following steps:
(1) two chlorine making beating: the water that adds 1450-1550KG in the diazonium bucket, the hydrochloric acid that adds again 265-295KG, described concentration of hydrochloric acid is 27-34%, two chlorine of 170-190KG are dropped in the diazonium bucket, and the stirring button of turn on agitator, carry out stirring to pulp, and add defoamer 5-10KG, beating time is at least 1 hour, in the situation that stir, adds ice cube, and the feed liquid in the diazonium bucket is cooled to below 0 ℃;
(2) diazotization, add in the diazonium bucket fast with in the sodium nitrite solution of 100-105KG is in 2min, and the concentration of described Sodium Nitrite is 32-42%, in the situation that stir, keeps feed temperature below 5 ℃, and keep the reaction times at 60-90min,
Drop into the auxiliary agent of 8-12KG, carry out the elimination of impurity, stirring 3-10min below 5 ℃, add water, make the cumulative volume in the diazonium bucket reach 2700-2850L, add thionamic acid to remove unnecessary Sodium Nitrite, and utilize the KI starch test paper to test, obtain finally diazo liquid;
(3) stop stirring, carry out suction strainer, during suction strainer, diazo liquid is filtered by cloth bag.
As preferably, described auxiliary agent is diatomite.After adopting above-mentioned preferred version, diatomite is a kind of siliceous rock, diatomite has special vesicular structure, have that fine and smooth, loose, quality is light, porous, water-absorbent, absorption property is strong and perviousness is strong physical property, can effectively remove the impurity in feed liquid, and diatomite is nontoxic, and pH is neutral, can not damage environment.
As preferably, described defoamer is polyvalent alcohol.After adopting above-mentioned preferred version, the better effects if of the froth breaking of polyvalent alcohol.
As preferably, the input amount of described hydrochloric acid is 275-285KG, and the concentration of hydrochloric acid is 28-32%.After adopting above-mentioned preferred version, the salt concn optimum, instead would not produce toxic gas.
As preferably, the input amount of described pair of chlorine is 175-185KG.After adopting above-mentioned preferred version, the reaction of two chlorine is the most appropriate, and toxic gas produces minimum.
As preferably, the Sodium Nitrite in described step (2) drops in the diazonium bucket fast in 1min.After adopting above-mentioned preferred version, caking phenomenon easily occurs in sodium nitrite solution, therefore needs fast with its input, in in 1min, it is put in the diazonium bucket, can effectively avoid the caking of nitrite, react more even, be not easy to produce the toxic gases such as nitrogen protoxide and nitrogen peroxide.
As preferably, the cloth bag in described step (3) is placed in a container, and described diazo liquid enters sealed vessel and enters cloth bag by the pipeline that is communicated with container, and after Bag filter, filtrate is derived by the outlet conduit on encloses container.After adopting above-mentioned preferred version, the filtration of diazo liquid is more comprehensive, and the diazo liquid filtrate that obtains is purer.
As preferably, the ice cube that adds in described step (1) is broken ice cube.After adopting above-mentioned preferred version, the contact area of the feed liquid in trash ice and diazonium bucket is larger, and cooling-down effect is better.
The preparation technology of the diazo liquid of permanent yellow G of the present invention does not have unnecessary two chlorine in the proportioning of two chlorine and hydrochloric acid, can avoid two chlorine to occur from even reaction, simultaneously, when two chlorine and hydrochloric acid reaction, feed temperature is down to below 0 ℃, and two chlorine can produce nitrogen protoxide and nitrogen dioxide gas with hydrochloric acid reaction the time, temperature is higher, it is more that toxic gas produces, and after arranging below 0 ℃, the toxic gas of generation is fewer.
Embodiment
Embodiment 1
(1) two chlorine making beating: add the water of 1500KG in the diazonium bucket, then to add the hydrochloric acid of 275KG, concentration of hydrochloric acid be 30%, two chlorine of 185KG are dropped in the diazonium bucket, and two chlorine are the 3-3-dichlorobenzidine hydrochloride, the stirring button of turn on agitator, carry out stirring to pulp, and to add defoamer 9KG, defoamer be polyvalent alcohol, 1,4 one butyleneglycols, beating time is 2 hours, in the situation that stir, adds broken ice cube, makes the feed liquid in the diazonium bucket be cooled to 0 ℃;
(2) diazotization, add in the diazonium bucket fast with in the sodium nitrite solution of 100KG is in 2min, and the concentration of Sodium Nitrite is 40%, in the situation that stir, keeps feed temperature at 4 ℃, and keep the reaction times at 80min,
Drop into the diatomite auxiliary agent of 10KG, carry out the elimination of impurity, stirring 8min below 5 ℃, add water, make the cumulative volume in the diazonium bucket reach 2700L, add thionamic acid to remove unnecessary Sodium Nitrite, and utilizing the KI starch test paper to test, test paper is little blueness, obtains finally diazo liquid;
(3) stop stirring, carry out suction strainer, during suction strainer, diazo liquid is filtered by cloth bag.Cloth bag is placed in a container, and described diazo liquid enters sealed vessel and enters cloth bag by the pipeline that is communicated with container, and after Bag filter, filtrate is derived by the outlet conduit on encloses container.
Embodiment 2
(1) two chlorine making beating: add the water of 1500KG in the diazonium bucket, then to add the hydrochloric acid of 280KG, concentration of hydrochloric acid be 31%, two chlorine of 180KG are dropped in the diazonium bucket, two chlorine are the 3-3-dichlorobenzidine hydrochloride, and the stirring button of turn on agitator, carry out stirring to pulp, and add defoamer 8KG, defoamer is polyvalent alcohol, neopentyl glycol, and beating time is 3 hours, add broken ice cube in the situation that stir, make the feed liquid in the diazonium bucket be cooled to 0 ℃;
(2) diazotization, add in the diazonium bucket fast with in the sodium nitrite solution of 103KG is in 2min, and the concentration of Sodium Nitrite is 37%, in the situation that stir, keeps feed temperature at 4 ℃, and keep the reaction times at 80min,
Drop into the diatomite auxiliary agent of 10KG, carry out the elimination of impurity, at 3 ℃, stir 10min, add water, make the cumulative volume in the diazonium bucket reach 2800L, add thionamic acid to remove unnecessary Sodium Nitrite, and utilizing the KI starch test paper to test, test paper is little blueness, obtains finally diazo liquid;
(3) stop stirring, carry out suction strainer, during suction strainer, diazo liquid is filtered by cloth bag.Cloth bag is placed in a container, and diazo liquid enters sealed vessel and enters cloth bag by the pipeline that is communicated with container, and after Bag filter, filtrate is derived by the outlet conduit on encloses container.
Embodiment 3
(1) two chlorine making beating: add the water of 1550KG in the diazonium bucket, then to add the hydrochloric acid of 295KG, concentration of hydrochloric acid be 27%, two chlorine of 190KG are dropped in the diazonium bucket, and two chlorine are the 3-3-dichlorobenzidine hydrochloride, the stirring button of turn on agitator, carry out stirring to pulp, and to add defoamer 10KG, defoamer be polyvalent alcohol, l, the 6-hexylene glycol, beating time is 3 hours, in the situation that stir, adds broken ice cube, makes the feed liquid in the diazonium bucket be cooled to-5 ℃;
(2) diazotization, add in the diazonium bucket fast with in the sodium nitrite solution of 104KG is in 2min, and the concentration of described Sodium Nitrite is 41%, in the situation that stir, keeps feed temperature at 3 ℃, and keep the reaction times at 90min,
Drop into the diatomite auxiliary agent of 12KG, carry out the elimination of impurity, at 3 ℃, stir 10min, add water, make the cumulative volume in the diazonium bucket reach 2850L, add thionamic acid to remove unnecessary Sodium Nitrite, and utilizing the KI starch test paper to test, test paper is little blueness, obtains finally diazo liquid;
(3) stop stirring, carry out suction strainer, during suction strainer, diazo liquid is filtered by cloth bag.Cloth bag is placed in a container, and described diazo liquid enters sealed vessel and enters cloth bag by the pipeline that is communicated with container, and after Bag filter, filtrate is derived by the outlet conduit on encloses container.
Embodiment 4
(1) two chlorine making beating: add the water of 1450KG in the diazonium bucket, then to add the hydrochloric acid of 265KG, concentration of hydrochloric acid be 34%, two chlorine of 170KG are dropped in the diazonium bucket, two chlorine are the 3-3-dichlorobenzidine hydrochloride, and the stirring button of turn on agitator, carry out stirring to pulp, and add defoamer 5KG, defoamer is polyvalent alcohol, and ethylene glycol, beating time are 1 hour, add broken ice cube in the situation that stir, make the feed liquid in the diazonium bucket be cooled to 0 ℃;
(2) diazotization, add in the diazonium bucket fast with in the sodium nitrite solution of 100KG is in 2min, and the concentration of described Sodium Nitrite is 42%, in the situation that stir, keeps feed temperature at 5 ℃, and keep the reaction times at 60min,
Drop into the diatomite auxiliary agent of 8KG, carry out the elimination of impurity, at 5 ℃, stir 3min, add water, make the cumulative volume in the diazonium bucket reach 2700L, add thionamic acid to remove unnecessary Sodium Nitrite, and utilizing the KI starch test paper to test, test paper is little blueness, obtains finally diazo liquid;
(3) stop stirring, carry out suction strainer, during suction strainer, diazo liquid is filtered by cloth bag.Cloth bag is placed in a container, and described diazo liquid enters sealed vessel and enters cloth bag by the pipeline that is communicated with container, and after Bag filter, filtrate is derived by the outlet conduit on encloses container.
Embodiment 5
(1) two chlorine making beating: add the water of 1520KG in the diazonium bucket, then to add the hydrochloric acid of 272KG, concentration of hydrochloric acid be 31%, two chlorine of 180KG are dropped in the diazonium bucket, and two chlorine are the 3-3-dichlorobenzidine hydrochloride, the stirring button of turn on agitator, carry out stirring to pulp, and to add defoamer 9KG, defoamer be polyvalent alcohol, 1, the 2-propylene glycol, beating time is at least 1 hour, in the situation that stir, adds broken ice cube, and the feed liquid in the diazonium bucket is cooled to below 0 ℃;
(2) diazotization, add in the diazonium bucket fast with in the sodium nitrite solution of 104KG is in 2min, and the concentration of Sodium Nitrite is 38%, in the situation that stir, keeps feed temperature below 5 ℃, and keep the reaction times at 70min,
Drop into the diatomite auxiliary agent of 10KG, carry out the elimination of impurity, at 4 ℃, stir 4min, add water, make the cumulative volume in the diazonium bucket reach 2800L, add thionamic acid to remove unnecessary Sodium Nitrite, and utilizing the KI starch test paper to test, test paper is little blueness, obtains finally diazo liquid;
(3) stop stirring, carry out suction strainer, during suction strainer, diazo liquid is filtered by cloth bag.Cloth bag is placed in a container, and described diazo liquid enters sealed vessel and enters cloth bag by the pipeline that is communicated with container, and after Bag filter, filtrate is derived by the outlet conduit on encloses container.
Embodiment 6
(1) two chlorine making beating: add the water of 1455KG in the diazonium bucket, then to add the hydrochloric acid of 265KG, concentration of hydrochloric acid be 28%, two chlorine of 175KG are dropped in the diazonium bucket, two chlorine are the 3-3-dichlorobenzidine hydrochloride, and the stirring button of turn on agitator, carry out stirring to pulp, and add defoamer 6KG, defoamer is polyvalent alcohol, methyl propanediol, and beating time is 1 hour, add broken ice cube in the situation that stir, make the feed liquid in the diazonium bucket be cooled to-2 ℃;
(2) diazotization, add in the diazonium bucket fast with in the sodium nitrite solution of 100-105KG is in 2min, and the concentration of Sodium Nitrite is 33%, in the situation that stir, keeps feed temperature at 4 ℃, and keep the reaction times at 65min,
Drop into the diatomite auxiliary agent of 8KG, carry out the elimination of impurity, at 4 ℃, stir 5min, add water, make the cumulative volume in the diazonium bucket reach 2750L, add thionamic acid to remove unnecessary Sodium Nitrite, and utilizing the KI starch test paper to test, test paper is little blueness, obtains finally diazo liquid;
(3) stop stirring, carry out suction strainer, during suction strainer, diazo liquid is filtered by cloth bag.Cloth bag is placed in a container, and described diazo liquid enters sealed vessel and enters cloth bag by the pipeline that is communicated with container, and after Bag filter, filtrate is derived by the outlet conduit on encloses container.
Claims (8)
1. the preparation technology of the diazo liquid of a permanent yellow G is characterized in that comprising the following steps:
(1) two chlorine making beating: the water that adds 1450-1550KG in the diazonium bucket, the hydrochloric acid that adds again 265-295KG, described concentration of hydrochloric acid is 27-34%, two chlorine of 170-190KG are dropped in the diazonium bucket, and the stirring button of turn on agitator, carry out stirring to pulp, and add defoamer 5-10KG, beating time is at least 1 hour, in the situation that stir, adds ice cube, and the feed liquid in the diazonium bucket is cooled to below 0 ℃;
(2) diazotization, add in the diazonium bucket fast with in the sodium nitrite solution of 100-105KG is in 2min, and the concentration of described Sodium Nitrite is 32-42%, in the situation that stir, keeps feed temperature below 5 ℃, and keep the reaction times at 60-90min,
Drop into the auxiliary agent of 8-12KG, carry out the elimination of impurity, stirring 3-10min below 5 ℃, add water, make the cumulative volume in the diazonium bucket reach 2700-2850L, add thionamic acid to remove unnecessary Sodium Nitrite, and utilize the KI starch test paper to test, obtain finally diazo liquid;
(3) stop stirring, carry out suction strainer, during suction strainer, diazo liquid is filtered by cloth bag.
2. the preparation technology of the diazo liquid of permanent yellow G according to claim 1, it is characterized in that: described auxiliary agent is diatomite.
3. the preparation technology of the diazo liquid of permanent yellow G according to claim 1, it is characterized in that: described defoamer is polyvalent alcohol.
4. the preparation technology of the diazo liquid of permanent yellow G according to claim 1, it is characterized in that: the input amount of described hydrochloric acid is 275-285KG, the concentration of hydrochloric acid is 28-32%.
5. the preparation technology of the diazo liquid of permanent yellow G according to claim 1, it is characterized in that: the input amount of described pair of chlorine is 175-185KG.
6. the preparation technology of the diazo liquid of permanent yellow G according to claim 1 is characterized in that: the Sodium Nitrite in described step (2) drops in the diazonium bucket fast in 1min.
7. the preparation technology of the diazo liquid of permanent yellow G according to claim 1, it is characterized in that: the cloth bag in described step (3) is placed in a container, described diazo liquid enters sealed vessel and enters cloth bag by the pipeline that is communicated with container, after Bag filter, filtrate is derived by the outlet conduit on encloses container.
8. the preparation technology of the diazo liquid of permanent yellow G according to claim 1 is characterized in that: the ice cube that adds in described step (1) is broken ice cube.
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| CN2013103295467A CN103396678A (en) | 2013-07-31 | 2013-07-31 | Process for preparing heavy nitrogen solution of permanent yellow G |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002363433A (en) * | 2001-06-11 | 2002-12-18 | Toyo Ink Mfg Co Ltd | Method for pigment yellow 14 production and use thereof |
| JP2003003085A (en) * | 2001-06-25 | 2003-01-08 | Toyo Ink Mfg Co Ltd | Production method for pigment-yellow 14 and its application |
| CN102719114A (en) * | 2012-05-29 | 2012-10-10 | 吴江市屯村颜料厂 | Method for preparing permanent yellow G |
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2013
- 2013-07-31 CN CN2013103295467A patent/CN103396678A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002363433A (en) * | 2001-06-11 | 2002-12-18 | Toyo Ink Mfg Co Ltd | Method for pigment yellow 14 production and use thereof |
| JP2003003085A (en) * | 2001-06-25 | 2003-01-08 | Toyo Ink Mfg Co Ltd | Production method for pigment-yellow 14 and its application |
| CN102719114A (en) * | 2012-05-29 | 2012-10-10 | 吴江市屯村颜料厂 | Method for preparing permanent yellow G |
Non-Patent Citations (1)
| Title |
|---|
| 周学良等: "《精细化工产品手册-颜料》", 30 April 2002 * |
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Application publication date: 20131120 |