CN1587323A - Process for two-step producing iron oxide red and iron oxide black and organic products - Google Patents
Process for two-step producing iron oxide red and iron oxide black and organic products Download PDFInfo
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- CN1587323A CN1587323A CN 200410060649 CN200410060649A CN1587323A CN 1587323 A CN1587323 A CN 1587323A CN 200410060649 CN200410060649 CN 200410060649 CN 200410060649 A CN200410060649 A CN 200410060649A CN 1587323 A CN1587323 A CN 1587323A
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Abstract
The two-step process of producing iron oxide red, iron oxide black and organic product includes the first reduction step of organic material, reductant and water in the ratio of 1 to 0-0.39 to 0-0.17 in a reactor, with excessive organic material being always maintained; the first filtering, mixing slurry, sieving, water washing, the second filtering and drying to prepare iron oxide red; the second reduction step of organic material, reductant and water in the ratio of 1 to 0.39-30 to 0.17-100 in the filtrate from the first filtering in the reactor, with the excessive reductant being always maintained; the sieving, water washing, filtering and drying to prepare iron oxide black and organic product.
Description
Technical field
The present invention relates to the production method of a kind of red iron oxide and iron oxide black, the method for particularly a kind of two-step approach production red iron oxide, iron oxide black and organic products.
Background technology
Conventional oxidation iron pigment production technology adds sour dissolving, oxidation, adds the preparation of alkali neutralization precipitation with iron, acid consumpting alkali, and the cost height easily causes environmental pollution; It is a kind of traditional organic products manufacturing process that reduction method is produced organic products, as by amines preparation by reducing aromatic nitro-compound, prepares phenol etc. by quinones.This technology has characteristics such as technical process is simple, low for equipment requirements, side reaction is few, but owing to produce a large amount of iron mud behind the iron powder reducing, its grade is low, and is normal discarded, easily causes the wasting of resources and environmental pollution.
Summary of the invention
Purpose of the present invention is exactly the method that a kind of two-step approach production red iron oxide, iron oxide black and organic products will be provided, and adopt red iron oxide, the iron oxide black excellent property of this method preparation, and processing cost is cheap.
The object of the present invention is achieved like this: the method for a kind of two-step approach production red iron oxide, iron oxide black and organic products may further comprise the steps:
(a) reduction: with organic raw material, reductive agent, water is 1 by weight: the ratio of 0-0.39: 0-0.17 drops in the reactor, temperature of reaction is 50 ℃-100 ℃ under the normal pressure, stirs mixing speed 10-120 rev/min 0.5-12 hour, it is excessive to remain organic raw material in the reaction
(b) once filter: the suspension filtered with (a) reduction reaction generates, obtain solid formation A, liquor B,
(c) size mixing, sieve: solid formation A is added add water to the surge tank and size mixing, dispersed with stirring under the normal temperature and pressure, mixing speed is 10-60 rev/min, and the suspension after sizing mixing is sieved, sieve number is 300 orders-600 orders,
(d) washing: screen underflow pump that will (c) step is to water washing tank, and it is colourless to the upper strata clear liquid to add the water cleaning,
(e) secondary filtration: with (d) step washing suspension filtered, obtain solid formation C,
(f) drying: solid formation C is carried out drying, the red iron oxide finished product, drying temperature is at 50 ℃-300 ℃, 0.5-30 hour time of drying,
(g) secondary reduction: be 1 by weight in organic raw material, reductive agent, water in the once filtering liquor B of (b) step: the ratio of 0.39-30: 0.17-100 drops in the reactor, temperature of reaction is 50 ℃-100 ℃ under the normal pressure, stirred 0.5-12 hour, mixing speed 10-120 rev/min, it is excessive to remain reductive agent in the reaction
(h) filter: the suspension filtered with (g) reduction reaction generates, obtain solid formation D, filtrate E,
(i) size mixing, sieve: solid formation D is added add water to the surge tank and size mixing, dispersed with stirring under the normal temperature and pressure, mixing speed is 10-60 rev/min, and the suspension after sizing mixing sieves, and sieve number is the 300-600 order,
(j) washing: to water washing tank, it is colourless to the upper strata clear liquid to add the water cleaning with (i) step screen underflow pump,
(k) filter: with (j) step washing suspension filtered, obtain solid formation F,
(l) drying: solid formation F is carried out drying, the iron oxide black finished product, drying temperature is at 50 ℃-300 ℃, 0.5-30 hour time of drying.
Wherein the reductive agent described in step (a), the step (g) is an iron powder.
Wherein the reductive agent described in step (a), the step (g) is the mixture of iron powder and ferric oxide, and weight ratio is 1: 0-10, ferrous iron content palpus 〉=35% in the ferric oxide.
Wherein the reductive agent described in step (a), the step (g) is a ferric oxide, ferrous iron content palpus 〉=35% in the ferric oxide.
Wherein the solid formation A described in step (b), the step (c) is that major ingredient is the iron mud of ferric oxide.
Wherein the liquor B described in step (b), the step (g) is the mixture of the intact organic raw material of unreacted, water, organic products.
Wherein the solid formation C described in step (f), the step (g) is that major ingredient is the iron mud of ferric oxide.
Wherein the solid formation D described in the step (h) is that major ingredient is the iron mud of Z 250 and the mixture of the reductive agent that unreacted finishes.
Wherein the filtrate E described in the step (h) is the mixture of water, organic products.
Wherein the solid formation F described in step (k), the step (l) is that major ingredient is the iron mud of Z 250.
Wherein the organic raw material described in step (a), (g) is aromatic nitro compound or quinones.
Adopt the existing conventional method to produce organic products with filtered liquid E, organic products is aminated compounds or phenolic compound.
The method of two-step approach production red iron oxide provided by the invention, iron oxide black and organic products, the iron powder that can utilize reduction reaction to produce is raw material, realized utilization of waste material, reduced environmental pollution, and red iron oxide, iron oxide black by the present invention's preparation are functional, meet relevant national standard.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples.
Fig. 1 is a process flow sheet of the present invention.
Fig. 1 double as Figure of abstract.
Embodiment
As shown in Figure 1, the method for a kind of two-step approach production red iron oxide, iron oxide black and organic products may further comprise the steps:
(a) reduction: with organic raw material, reductive agent, water is 1 by weight: the ratio of 0-0.39: 0-0.17 drops in the reactor, temperature of reaction is 50 ℃-100 ℃ under the normal pressure, stirs mixing speed 10-120 rev/min 0.5-12 hour, it is excessive to remain organic raw material in the reaction
(b) once filter: the suspension filtered with (a) reduction reaction generates, obtain solid formation A, liquor B,
(c) size mixing, sieve: solid formation A is added add water to the surge tank and size mixing, dispersed with stirring under the normal temperature and pressure, mixing speed is 10-60 rev/min, and the suspension after sizing mixing is sieved, sieve number is 300 orders-600 orders,
(d) washing: screen underflow pump that will (c) step is to water washing tank, and it is colourless to the upper strata clear liquid to add the water cleaning,
(e) secondary filtration: with (d) step washing suspension filtered, obtain solid formation C,
(f) drying: solid formation C is carried out drying, the red iron oxide finished product, drying temperature is at 50 ℃-300 ℃, 0.5-30 hour time of drying,
(g) secondary reduction: be 1 by weight in organic raw material, reductive agent, water in the once filtering liquor B of (b) step: the ratio of 0.39-30: 0.17-100 drops in the reactor, temperature of reaction is 50 ℃-100 ℃ under the normal pressure, stirred 0.5-12 hour, mixing speed 10-120 rev/min, it is excessive to remain reductive agent in the reaction
(h) filter: the suspension filtered with (g) reduction reaction generates, obtain solid formation D, filtrate E,
(i) size mixing, sieve: solid formation D is added add water to the surge tank and size mixing, dispersed with stirring under the normal temperature and pressure, mixing speed is 10-60 rev/min, and the suspension after sizing mixing sieves, and sieve number is the 300-600 order,
(j) washing: to water washing tank, it is colourless to the upper strata clear liquid to add the water cleaning with (i) step screen underflow pump,
(k) filter: with (j) step washing suspension filtered, obtain solid formation F,
(l) drying: solid formation F is carried out drying, the iron oxide black finished product, drying temperature is at 50 ℃-300 ℃, 0.5-30 hour time of drying.
Wherein the reductive agent described in step (a), the step (g) is an iron powder.
Wherein the reductive agent described in step (a), the step (g) is the mixture of iron powder and ferric oxide, and weight ratio is 1: 0-10, ferrous iron content palpus 〉=35% in the ferric oxide.
Wherein the reductive agent described in step (a), the step (g) is a ferric oxide, ferrous iron content palpus 〉=35% in the ferric oxide.
Wherein the solid formation A described in step (b), the step (c) is that major ingredient is the iron mud of ferric oxide.
Wherein the liquor B described in step (b), the step (g) is the mixture of the intact organic raw material of unreacted, water, organic products.
Wherein the solid formation C described in step (f), the step (g) is that major ingredient is the iron mud of ferric oxide.
Wherein the solid formation D described in the step (h) is that major ingredient is the iron mud of Z 250 and the mixture of the reductive agent that unreacted finishes.
Wherein the filtrate E described in the step (h) is the mixture of water, organic products.
Wherein the solid formation F described in step (k), the step (l) is that major ingredient is the iron mud of Z 250.
Wherein the organic raw material described in step (a), (g) is aromatic nitro compound or quinones.
Organic products is aminated compounds or phenolic compound.
Embodiment 1:
10% para benzoquinone solution 770ml, 300ml water are joined respectively in the 2000ml container, and turn on agitator stirs,
Heat temperature raising is again to wherein slowly adding the 20g iron powder.To go out pulp suspension once filters, get filter cake 35g, filtrate 360ml, filter cake adds water-dispersion, and the suspension after disperseing is sieved after (mesh size is less than 45 microns), adding water cleans, colourless to the upper strata clear liquid until washing, secondary filtration is put into CLS101-E type baking oven with solid formation then, in 65 ℃-75 ℃ oven dry, grinding, just get finished product red iron oxide 22g.Detecting tinting strength is 100% (with the standard specimen ratio), Fe
2O
3Content 95%.150g iron powder, 50ml water are added in the reduction pot, and dispersed with stirring, intensification are with 360ml filtrate, 10% para benzoquinone solution 500ml, be added in the reduction pot, after after react the suspension of generation being sieved, add the water cleaning, colourless until washing to the upper strata clear liquid, secondary filtration is put into CLS101-E type baking oven with solid formation then, oven dry in about 95 ℃, grind, just get finished product iron oxide black 96g, detecting tinting strength is 105% (with the standard specimen ratio), Fe
3O
4Content 94%.
Embodiment 2:
98% nitrobenzene solution 80ml, 900ml water are joined respectively in the 2000ml container, the turn on agitator dispersed with stirring, heat temperature raising is again to wherein slowly adding the iron scale (FeII content is 64%) that 45g iron and steel Re Zha factory produces.To go out pulp suspension 1000ml once filters, get filter cake 110g, filtrate 930ml, filter cake add the 150ml water-dispersion, after the suspension after disperseing is sieved, adding water cleans, colourless to the upper strata clear liquid until washing, secondary filtration is put into CLS101-E type baking oven with solid formation then, oven dry in about 95 ℃, grinding just get finished product red iron oxide 86g.Detecting tinting strength is 105% (with the standard specimen ratio), Fe
2O
3Content 95%.350g fine iron breeze (FeII content is 40%), 280ml water are added in the reduction pot, and dispersed with stirring, intensification are with 930ml filtrate, 98% nitrobenzene solution 50ml, be added in the reduction pot, after after react the suspension of generation being sieved, add the water cleaning, colourless until washing to the upper strata clear liquid, secondary filtration is put into CLS101-E type baking oven with solid formation then, oven dry in about 95 ℃, grind, just get finished product iron oxide black 106g, detecting tinting strength is 100% (with the standard specimen ratio), Fe
3O
4Content 92%.
Embodiment 3:
98% nitrobenzene solution 400L, 4500L water are added 7m respectively
3In the reduction pot, the turn on agitator dispersed with stirring, heat temperature raising is again to wherein slowly adding 220Kg fine iron breeze (FeII content is 68%).To go out the about 5m of pulp suspension
3Carry out filter press one time, get filter cake 600Kg, filtrate 4.5m
3, filter cake adds the 600L water-dispersion, after the suspension after disperseing is sieved, add water and clean, colourless until washing to the upper strata clear liquid, secondary filter press then, it is dry that solid formation is put into industrial baking oven, and oven dry in about 95 ℃, grinding just get finished product red iron oxide 450Kg.Detecting tinting strength is 100% (with the standard specimen ratio), Fe
2O
3Content 96%.1.8 tons of iron scales (FeII content is 68%), 1.5m with the generation of iron and steel Re Zha factory
3Water is added in the reduction pot, and dispersed with stirring, intensification are with 4.5m
3Filtrate, 98% nitrobenzene solution 250L, be added in the reduction pot, after after react the suspension of generation being sieved, add the water cleaning, colourless until washing to the upper strata clear liquid, Plate Filtration is put into industrial baking oven drying, oven dry in about 90 ℃ with solid formation then, grind, just get finished product iron oxide black 330Kg, detecting tinting strength is 100% (with the standard specimen ratio), Fe
3O
4Content 95%.
Claims (12)
1, the method for a kind of two-step approach production red iron oxide, iron oxide black and organic products is characterized in that: may further comprise the steps:
(a) reduction: with organic raw material, reductive agent, water is 1 by weight: the ratio of 0-0.39: 0-0.17 drops in the reactor, temperature of reaction is 50 ℃-100 ℃ under the normal pressure, stirs mixing speed 10-120 rev/min 0.5-12 hour, it is excessive to remain organic raw material in the reaction
(b) once filter: the suspension filtered with (a) reduction reaction generates, obtain solid formation A, liquor B,
(c) size mixing, sieve: solid formation A is added add water to the surge tank and size mixing, dispersed with stirring under the normal temperature and pressure, mixing speed is 10-60 rev/min, and the suspension after sizing mixing is sieved, sieve number is 300 orders-600 orders,
(d) washing: screen underflow pump that will (c) step is to water washing tank, and it is colourless to the upper strata clear liquid to add the water cleaning,
(e) secondary filtration: with (d) step washing suspension filtered, obtain solid formation C,
(f) drying: solid formation C is carried out drying, the red iron oxide finished product, drying temperature is at 50 ℃-300 ℃, 0.5-30 hour time of drying,
(g) secondary reduction: be 1 by weight in organic raw material, reductive agent, water in the once filtering liquor B of (b) step: the ratio of 0.39-30: 0.17-100 drops in the reactor, temperature of reaction is 50 ℃-100 ℃ under the normal pressure, stirred 0.5-12 hour, mixing speed 10-120 rev/min, it is excessive to remain reductive agent in the reaction
(h) filter: the suspension filtered with (g) reduction reaction generates, obtain solid formation D, filtrate E,
(i) size mixing, sieve: solid formation D is added add water to the surge tank and size mixing, dispersed with stirring under the normal temperature and pressure, mixing speed is 10-60 rev/min, and the suspension after sizing mixing sieves, and sieve number is the 300-600 order,
(j) washing: to water washing tank, it is colourless to the upper strata clear liquid to add the water cleaning with (i) step screen underflow pump,
(k) filter: with (j) step washing suspension filtered, obtain solid formation F,
(l) drying: solid formation F is carried out drying, the iron oxide black finished product, drying temperature is at 50 ℃-300 ℃, 0.5-30 hour time of drying.
2, the method for a kind of two-step approach production red iron oxide according to claim 1, iron oxide black and organic products, it is characterized in that: wherein the reductive agent described in step (a), the step (g) is an iron powder.
3, the method for a kind of two-step approach production red iron oxide according to claim 1, iron oxide black and organic products, it is characterized in that: wherein the reductive agent described in step (a), the step (g) is the mixture of iron powder and ferric oxide, weight ratio is 1: 0-10, ferrous iron content palpus 〉=35% in the ferric oxide.
4, the method for a kind of two-step approach production red iron oxide according to claim 1, iron oxide black and organic products, it is characterized in that: wherein the reductive agent described in step (a), the step (g) is a ferric oxide, ferrous iron content palpus 〉=35% in the ferric oxide.
5, the method for a kind of two-step approach production red iron oxide according to claim 1, iron oxide black and organic products is characterized in that: wherein the solid formation A described in step (b), the step (c) is that major ingredient is the iron mud of ferric oxide.
6, the method for a kind of two-step approach production red iron oxide according to claim 1, iron oxide black and organic products is characterized in that: wherein the liquor B described in step (b), the step (g) is the mixture of the intact organic raw material of unreacted, water, organic products.
7, the method for a kind of two-step approach production red iron oxide according to claim 1, iron oxide black and organic products is characterized in that: wherein the solid formation C described in step (f), the step (g) is that major ingredient is the iron mud of ferric oxide.
8, the method for a kind of two-step approach production red iron oxide according to claim 1, iron oxide black and organic products is characterized in that: wherein the solid formation D described in the step (h) is that major ingredient is the iron mud of Z 250 and the mixture of the reductive agent that unreacted finishes.
9, the method for a kind of two-step approach production red iron oxide according to claim 1, iron oxide black and organic products, it is characterized in that: wherein the filtrate E described in the step (h) is the mixture of water, organic products.
10, the method for a kind of two-step approach production red iron oxide according to claim 1, iron oxide black and organic products is characterized in that: wherein the solid formation F described in step (k), the step (l) is that major ingredient is the iron mud of Z 250.
11, the method for a kind of two-step approach production red iron oxide according to claim 1, iron oxide black and organic products, it is characterized in that: wherein the organic raw material described in step (a), (g) is aromatic nitro compound or quinones.
12, according to the method for claim 1 or 9 described a kind of two-step approach production red iron oxides, iron oxide black and organic products, it is characterized in that: organic products is aminated compounds or phenolic compound.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106675097A (en) * | 2016-11-15 | 2017-05-17 | 广东荣高陶瓷有限公司 | Preparation method of pigment for ceramic body |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106675097A (en) * | 2016-11-15 | 2017-05-17 | 广东荣高陶瓷有限公司 | Preparation method of pigment for ceramic body |
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