CN102531017B - Carbonizer and method for producing nano calcium carbonate - Google Patents
Carbonizer and method for producing nano calcium carbonate Download PDFInfo
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- CN102531017B CN102531017B CN 201210060076 CN201210060076A CN102531017B CN 102531017 B CN102531017 B CN 102531017B CN 201210060076 CN201210060076 CN 201210060076 CN 201210060076 A CN201210060076 A CN 201210060076A CN 102531017 B CN102531017 B CN 102531017B
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 111
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 75
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 5
- 239000002002 slurry Substances 0.000 claims abstract description 271
- 238000003763 carbonization Methods 0.000 claims abstract description 183
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 162
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 108
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 108
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 108
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 58
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 58
- 230000012010 growth Effects 0.000 claims abstract description 41
- 230000032683 aging Effects 0.000 claims abstract description 40
- 238000006243 chemical reaction Methods 0.000 claims abstract description 39
- 238000003860 storage Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000013078 crystal Substances 0.000 claims abstract description 18
- 230000006911 nucleation Effects 0.000 claims abstract description 16
- 238000010899 nucleation Methods 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 230000003213 activating effect Effects 0.000 claims abstract description 4
- 238000005255 carburizing Methods 0.000 claims description 78
- 239000003153 chemical reaction reagent Substances 0.000 claims description 78
- 235000011089 carbon dioxide Nutrition 0.000 claims description 46
- 239000003795 chemical substances by application Substances 0.000 claims description 25
- 230000004913 activation Effects 0.000 claims description 23
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 14
- 230000015572 biosynthetic process Effects 0.000 claims description 14
- 239000006185 dispersion Substances 0.000 claims description 11
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 10
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 10
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 10
- 238000009825 accumulation Methods 0.000 claims description 7
- 239000013543 active substance Substances 0.000 claims description 7
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 235000019353 potassium silicate Nutrition 0.000 claims description 7
- 150000003839 salts Chemical class 0.000 claims description 7
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 7
- 239000002689 soil Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 230000003197 catalytic effect Effects 0.000 claims description 5
- 239000011575 calcium Substances 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 238000009826 distribution Methods 0.000 abstract description 13
- 238000005265 energy consumption Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 8
- 238000012544 monitoring process Methods 0.000 description 5
- 230000003698 anagen phase Effects 0.000 description 3
- 230000005587 bubbling Effects 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- FGRBYDKOBBBPOI-UHFFFAOYSA-N 10,10-dioxo-2-[4-(N-phenylanilino)phenyl]thioxanthen-9-one Chemical compound O=C1c2ccccc2S(=O)(=O)c2ccc(cc12)-c1ccc(cc1)N(c1ccccc1)c1ccccc1 FGRBYDKOBBBPOI-UHFFFAOYSA-N 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- JOHZPMXAZQZXHR-UHFFFAOYSA-N pipemidic acid Chemical compound N1=C2N(CC)C=C(C(O)=O)C(=O)C2=CN=C1N1CCNCC1 JOHZPMXAZQZXHR-UHFFFAOYSA-N 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
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Abstract
The invention discloses a carbonizer for producing nano calcium carbonate. The carbonizer comprises a calcium hydroxide blending tank, a calcium hydroxide slurry storage tank, a primary carbonization nucleation reactor, a primary carbonization growth reactor, a primary carbonization ageing tank, a secondary carbonization tubular reactor and a calcium hydroxide activating tank; and a slurry carbonization reaction tube and a carbon dioxide porous reaction tube which have two-end uninterrupted repeated arch structures are arranged in the primary carbonization nucleation reactor, the primary carbonization growth reactor and the secondary carbonization tubular reactor respectively. By the method for producing the nano calcium carbonate through the carbonizer, the calcium carbonate can be produced by the nucleation stage and the growth stage, and is controlled stepwise, the reaction degree of the whole carbonization process can be monitored, the nano calcium carbonate with uniform particle size distribution, regular crystal structures and stable quality can be produced, and the invention has the advantages of small equipment investment, short carbonization time, low energy consumption and the like.
Description
Technical field
The present invention relates to a kind of equipment of producing nano-calcium carbonate, particularly relate to a kind of novel carbonization reactor and method of continuous production nano-calcium carbonate.
Background technology
Carburizing reagent is to carry out in a gas, liquid, solid three-phase reaction system, wherein relates to dissolving, the carbon dioxide gas bulk absorption of calcium hydroxide solid, precipitation and the calcium carbonate particles nucleating growth process of calcium carbonate." carborization " is to prepare the method that generally adopts in the calcium carbonate at present both at home and abroad, and the carbonization process of calcium hydroxide and carbon dioxide reaction is a most key step.At present both at home and abroad the carbonization method of comparative maturity has four kinds: intermittently bubbling style carborization, intermittently stirring-type carborization, multistage spray carbonation method and hypergravity formula carborization intermittently continuously.Wherein from the cost aspect, preceding two kinds of methods are hanged down two kinds of method height then; From investment situation, also be the low two kinds of method height then of preceding two kinds of methods.So it is main producing the many two kinds of methods in the past of nano-calcium carbonate both at home and abroad, intermittently the bubbling style carborization, intermittently the stirring-type carborization is will be added with to lead to after the calcium hydroxide slurry refrigeration of additives such as dispersion agent and crystal formation directed agents stirrer is housed or does not adorn in the carbonating tower of stirrer, lead to carbon dioxide at the bottom of tower, calcium hydroxide and carbon dioxide reaction generate precipitation of calcium carbonate.The variation of the crystal habit of factor affecting calcium carbonate such as because Gu calcium hydroxide and carbonic acid gas are the thermopositive reaction that gas-liquid-three contacts, gas distribution is inhomogeneous, the continuous rising of temperature of reaction.The weak point of these two kinds of carbonization modes is as follows: 1) the product crystal structure irregularity of Sheng Chaning has a very wide distribution with series-produced product cut size; 2) reaction times longer, the carbonic acid gas utilization ratio is low; 3) be difficult to realization to the complete monitoring of carbonization process, difficult realization control automatically; 4) calcium carbonate nucleation and growth phase are difficult to the particle diameter of control calcium carbonate at the row wherein time the with carburizing reagent, cause product fluctuation people.
Summary of the invention
The problem that the present invention need solve is that calcium carbonate nucleation and growth phase be not separately in the prior art, be difficult to the particle diameter of control calcium carbonate, cause product fluctuation people, this is designed a kind of continuous production, size distribution evenly, regular crystal forms, product favorable reproducibility, carbonization time weak point, carbonic acid gas utilization ratio height, calcium carbonate nucleation stage and growth phase control and can monitor the response situation of each particle in the whole carbonization process and carbonizer and the method for level of response step by step.
In order to arrive above-mentioned purpose in the limit, the technical solution used in the present invention is: a kind of carbonizer of producing nano-calcium carbonate, comprise the calcium hydroxide preparing pool, the calcium hydroxide slurry storage pool that is attached thereto, this carbonizer comprises that also an interconnective carbonization successively becomes nuclear reactor, a carbonization growth reactor, a carbonization ageing pond, secondary carbonization tubular reactor and calcium carbonate activation pond, a described carbonization becomes nuclear reactor to be connected with the slurries output terminal of calcium hydroxide slurry storage pool.
A described carbonization becomes to be provided with slurries ingress pipe, slurries carburizing reagent pipe and the discharge pipe that from top to bottom connects successively in the nuclear reactor; The one end mouth of pipe of described slurries ingress pipe extends to outside this reactor and is connected with the slurries output terminal of calcium hydroxide slurry storage pool by pipeline.
Be provided with from top to bottom the slurries ingress pipe that connects successively, slurries carburizing reagent pipe in the described carbonization growth reactor with the skill discharge pipe; The one end mouth of pipe of described slurries ingress pipe extends to outside this reactor and becomes the discharge pipe of nuclear reactor to be connected by pipeline with a carbonization, and described discharge pipe is connected by the slurries input terminus of pipeline with a carbonization ageing pond.
Be provided with slurries carburizing reagent pipe in the described secondary carbonization tubular reactor, the mouth of pipe of this slurries carburizing reagent Guan Yiduan extends to outside this reactor and is connected by the slurries output terminal of pipeline with a carbonization ageing pond, and the another port is stretched out in this reactor bottom and is connected in the calcium carbonate activation pond.
A described carbonization becomes in the slurries carburizing reagent pipe in nuclear reactor, carbonization growth reactor and the secondary carbonization tubular reactor to be provided with carbonic acid gas porous reaction pipe, and this carbonic acid gas porous reaction pipe is communicated with the carbonic acid gas input tube that is arranged at this reactor one side.
A described carbonization becomes the carbonic acid gas porous reaction pipe in nuclear reactor, carbonization growth reactor and the secondary carbonization tubular reactor to be provided be used to making the catalytic hole of carbonic acid gas and slurries.
Further, a described carbonization becomes the slurries ingress pipe in nuclear reactor, carbonization growth reactor and each reactor of secondary carbonization tubular reactor to be the two ends unremitting bow-shaped structural structure of answering continuously with slurries carburizing reagent pipe and carbonic acid gas porous reaction pipe.
Further, to become the bore of the discharge pipe in nuclear reactor, the carbonization growth reactor be 2 times of bore of slurries carburizing reagent pipe in a described carbonization.
A kind of method of utilizing above-mentioned carbonizer to produce nano-calcium carbonate, its step is as follows:
1) modulation of calcium hydroxide slurry:
The concentration of deployed calcium hydroxide slurry in the calcium hydroxide preparing pool, and in calcium hydroxide slurry, add crystal formation directed agents and dispersion agent sodium hexametaphosphate, and mixing and stirring;
2) storage of calcium hydroxide slurry:
Will be in the calcium hydroxide preparing pool deployed slurries be extracted in the calcium hydroxide slurry storage pool and store;
3) carbonization nucleation reaction treatment:
Slurries in the calcium hydroxide slurry storage pool are led to a carbonization become slurries ingress pipe in the nuclear reactor, and become carbonic acid gas input tube in the nuclear reactor to feed carbon dioxide through purifying treatment toward a carbonization, make slurries and carbon dioxide contact reacts in slurries carburizing reagent pipe, obtain calcium hydroxide and calcium carbonate mixing suspension, reacted slurries are discharged from the discharge pipe in this reactor;
4) a carbonization growth response is handled:
The reacted slurries of carbonization nucleation are led to the slurries ingress pipe in the carbonization growth reactor one time, and the carbonic acid gas input tube in carbonization growth reactor feeds the carbon dioxide through purifying treatment, make calcium hydroxide and carbon dioxide contact reacts in slurries carburizing reagent pipe in the slurries, obtain the nano-calcium carbonate slurries, reacted slurries are discharged from the discharge pipe of this reactor;
5) ageing is handled:
Slurries after the carbonization growth response are led in a carbonization ageing pond carry out ageing, remove the impurity in the nano-calcium carbonate slurries and make the particle diameter of nano-calcium carbonate even;
6) the secondary carburizing reagent is handled:
Slurries after ageing is handled have the calcium hydroxide of a small amount of accumulation of salt in the surface soil, slurries after a carbonization ageing pond ageing are extracted into the slurries carburizing reagent pipe of secondary carbonization tubular reactor, and the carbonic acid gas input tube in carbonization growth reactor feeds the carbon dioxide through purifying treatment, makes calcium hydroxide and carbon dioxide contact reacts in slurries carburizing reagent pipe in the slurries;
7) activation treatment:
To in secondary carbonization tubular reactor, lead to calcium carbonate activation pond by reacted nano-calcium carbonate slurries, and add tensio-active agent and handle;
8) dehydrate processing:
Slurries after the pond activation dewater with activating at calcium carbonate, drying treatment, obtain required nano-calcium carbonate calcium product.
In the described step 1), the mass concentration of the calcium hydroxide slurry of described allotment is
Described crystal formation directed agents is a kind of in magnesium chloride, sal epsom, the water glass, the crystal formation directed agents of adding and the quality of dispersion agent sodium hexametaphosphate be calcium hydroxide ten bases in the calcium hydroxide slurry the quality percentage composition 0.1%～2%.
In described step 3), step 4) and the step 6), the carbon dioxide that feeds in each carburizing reagent is the carbon dioxide of volumetric concentration 〉=20%.
In described step 3), step 1) and the step 6), carry out heat exchange by the outer water of the slurries in the slurries carburizing reagent pipe and pipe in each carburizing reagent, make the carbonization temperature control of each carburizing reagent between 10～45 ℃.
Compared with the prior art, the invention has the beneficial effects as follows: can continuously production size distribution evenly, very regular, the quality product of crystalline structure stabilized nano calcium carbonate very, have simultaneously that facility investment is little, carbonization time short, low power consumption and other advantages.
Description of drawings
Fig. 1 is the structural representation of carbonizer of the present invention;
Fig. 2 is the structural representation that a carbonization in the carbonizer of the present invention becomes nuclear reactor;
Fig. 3 is that a carbonization growth reactor in the carbonizer of the present invention is looked for structural representation;
Fig. 4 is the structural representation of the secondary carbonization tubular reactor in the carbonizer of the present invention
Embodiment
For the ease of those skilled in the art's understanding, below in conjunction with accompanying drawing and specific embodiment the present invention is done the further thin description in ocean, but specific embodiment is not done any restriction to the present invention.
As shown in Figure 1, a kind of carbonizer of producing nano-calcium carbonate, comprise by pipeline and become nuclear reactor 1, carbonization growth reactor 2, carbonization ageing pond 6, secondary carbonization tubular reactor 3 with pump interconnective calcium hydroxide preparing pool 1 successively, calcium hydroxide slurry storage pool 5, a carbonization, this carbonizer also comprises calcium carbonate activation pond 7, and the slurries carbonized tube 9 of secondary carbonization tubular reactor 3 is in calcium carbonate activation pond 7.
As accompanying drawing 1, shown in 2, a described carbonization becomes to be provided with the slurries ingress pipe 8 that from top to bottom connects successively in the nuclear reactor 1, slurries carburizing reagent pipe 9 and discharge pipe 10, the one end mouth of pipe of slurries ingress pipe 8 extends to outside this reactor and is connected with the slurries output terminal of calcium hydroxide slurry storage pool 5 by pipeline, discharge pipe 10 is positioned at the bottom of this reactor, and be provided with carbonic acid gas porous reaction pipe 12 in the pipeline that is connected pump is communicated with slurries carburizing reagent pipe 9, this carbonic acid gas porous reaction pipe 12 is communicated with the carbonic acid gas input tube 11 that is arranged at this reactor right side, and is provided be used to making the catalytic hole of carbonic acid gas and slurries.
Shown in accompanying drawing 1,3, a described carbonization growth reactor 2 becomes nuclear reactor 1 structure identical with a carbonization, be provided with the slurries ingress pipe 8, slurries carburizing reagent pipe 9 and the discharge pipe 10 that from top to bottom connect successively in this carbonization growth reactor 2, the one end mouth of pipe of slurries ingress pipe 8 extends to outside this reactor and becomes the discharge pipe 10 of nuclear reactor 1 to be connected by pipeline and a carbonization, and the discharge pipe 10 of a carbonization growth reactor 2 is connected with the slurries input terminus in a carbonization ageing pond 6.Be provided with carbonic acid gas porous reaction pipe 12 in the slurries carburizing reagent pipe 9, this carbonic acid gas porous reaction pipe 12 is communicated with the carbonic acid gas input tube 11 that is arranged at this reactor one side, and is provided be used to making the catalytic hole of carbonic acid gas and slurries.
Shown in accompanying drawing 1,4, be provided with slurries carburizing reagent pipe 9 and carbonic acid gas input tube 11 in the described secondary carbonization tubular reactor 3, be provided with carbonic acid gas porous reaction pipe 12 in slurries carburizing reagent pipe 9, described carbonic acid gas porous reaction pipe 9 is communicated with carbonic acid gas input tube 11 and is provided be used to making the catalytic hole of carbonic acid gas and slurries; The mouth of pipe of slurries carburizing reagent pipe 9 one ends of this secondary carbonization tubular reactor extends to that this reactor is outer to be connected with the slurries output terminal in a carbonization ageing pond 6 by He Dao, and the another port is stretched out in this reactor bottom and is connected to calcium carbonate and activates in the pond 7.
Wherein, a carbonization becomes the slurries ingress pipes 8 in nuclear reactor 1, carbonization growth reactor 2 and the secondary carbonization tubular reactor 3 to be the continuous unremitting repetition bow-shaped structural structure in two ends with slurries carburizing reagent pipe 9 and carbonic acid gas porous reaction pipe 12, and the bore of discharge pipe 10 is 2 times of bore of slurries carburizing reagent pipe 9.
A kind of method of utilizing above-mentioned carbonizer to produce nano-calcium carbonate, its step is as follows:
1) modulation of calcium hydroxide slurry:
The concentration of deployed calcium hydroxide slurry in the calcium hydroxide preparing pool, and in calcium hydroxide slurry, add crystal formation directed agents and dispersion agent sodium hexametaphosphate, and mixing and stirring;
2) storage of calcium hydroxide slurry:
Will be in the calcium hydroxide preparing pool deployed slurries be extracted in the calcium hydroxide slurry storage pool and store;
3) carbonization nucleation reaction treatment:
Slurries in the calcium hydroxide slurry storage pool are led to a carbonization become slurries ingress pipe in the nuclear reactor, and become carbonic acid gas input tube in the nuclear reactor to feed carbon dioxide through purifying treatment toward a carbonization, make slurries and carbon dioxide contact reacts in slurries carburizing reagent pipe, obtain calcium hydroxide and calcium carbonate mixing suspension, reacted slurries are discharged from the discharge pipe in this reactor;
4) a carbonization growth response is handled:
The reacted slurries of carbonization nucleation are led to the slurries ingress pipe in the carbonization growth reactor one time, and the carbonic acid gas input tube in carbonization growth reactor feeds the carbon dioxide through purifying treatment, make calcium hydroxide and carbon dioxide contact reacts in slurries carburizing reagent pipe in the slurries, obtain the nano-calcium carbonate slurries, reacted slurries are discharged from the discharge pipe of this reactor;
5) ageing is handled:
Slurries after the carbonization growth response are led in a carbonization ageing pond carry out ageing, remove the impurity in the nano-calcium carbonate slurries and make the particle diameter of nano-calcium carbonate even;
6) the secondary carburizing reagent is handled:
Slurries after ageing is handled have the calcium hydroxide of a small amount of accumulation of salt in the surface soil, slurries after a carbonization ageing pond ageing are extracted into the slurries carburizing reagent pipe of secondary carbonization tubular reactor, and the carbonic acid gas input tube in carbonization growth reactor feeds the carbon dioxide through purifying treatment, makes calcium hydroxide and carbon dioxide contact reacts in slurries carburizing reagent pipe in the slurries;
7) activation treatment:
To in secondary carbonization tubular reactor, lead to calcium carbonate activation pond by reacted nano-calcium carbonate slurries, and add tensio-active agent and handle;
8) dehydrate processing:
Slurries after the pond activation dewater with activating at calcium carbonate, drying treatment, obtain required nano-calcium carbonate calcium product.
In the described step 1), the mass concentration of the calcium hydroxide slurry of described allotment is 5%～15%; Described crystal formation directed agents is a kind of in magnesium chloride, sal epsom, the water glass, the crystal formation directed agents of adding and the quality of dispersion agent sodium hexametaphosphate be calcium hydroxide butt in the calcium hydroxide slurry the quality percentage composition 0.1%～2%.
In described step 3), step 4) and the step 6), the carbon dioxide that feeds in each carburizing reagent is the carbon dioxide of volumetric concentration 〉=20%, controls the speed of reaction of each carburizing reagent by the size of control flow of carbon dioxide gas amount.
In described step 3), step 1) and the step 6), carry out the carbonization temperature that each carburizing reagent is controlled in heat exchange by the outer water of the slurries in the slurries carburizing reagent pipe and pipe in each carburizing reagent, make the carbonization temperature control of each carburizing reagent between 10～45 ℃.
Adjusting calcium hydroxide mass concentration is 6%～15% calcium hydroxide slurry in the calcium hydroxide preparing pool, deployed back is stored calcium hydroxide slurry in the calcium hydroxide slurry storage pool into, the temperature of the calcium hydroxide slurry in the calcium hydroxide slurry storage pool is controlled between 10 ℃～30 ℃, and to add the quality percentage composition account for the calcium hydroxide butt be 0.1%～2% crystal formation directed agents magnesium chloride, sal epsom, wherein a kind of of water glass, add 0.1～2% dispersion agent sodium hexametaphosphate again, become to pump into calcium hydroxide slurry in the nuclear reactor toward a carbonization after the mixing and stirring, and become the carbon dioxide that feeding has purified in the nuclear reactor toward a carbonization, the volumetric concentration of carbonic acid gas 〉=20%, the carbon dioxide of feeding with in the continuous contact reacts of slurries carburizing reagent Guan Zhongyu slurries.
Size by control flow of carbon dioxide gas amount is controlled speed of reaction, the water outer by slurries in the slurries carburizing reagent pipe and pipe carries out heat exchange, the control carbonization temperature is between 10 ℃～30 ℃, by monitoring the viscosity variation of slurries in the slurries carburizing reagent pipe, controlling a carbonization nucleation reacting slurry viscosity is 800mpa.s～950mpa.s, when monitor when the carbonization slurry viscosity of layer 800mpa.s～950mpa.s at present the slurries carburizing reagent pipe of one deck stop logical carbon dioxide
Slurries after becoming the nuclear reactor internal reaction a carbonization are led to a carbonization grower, the temperature of a carbonization grower is controlled between 10 ℃～30 ℃, the carbon dioxide that feeds volumetric concentration 〉=20% of process purifying treatment carries out carbonization, make two ends unremitting slurries and the continuous contact reacts of carbon dioxide that repeats in the arched slurries carburizing reagent pipe continuously, reacted slurries flow out from the discharge pipe of a carbonization growth reactor bottom, resulting slurry pH value is 7～8, and particle diameter is about 30nm, size distribution is even, the nano-calcium carbonate slurries of good dispersity.
The nano-calcium carbonate slurries that become the nuclear reactor internal reaction to obtain a carbonization lead to a carbonization ageing pond ageing and after 1～6 day slurries are extracted in the slurries carburizing reagent pipe of secondary carbonization tubular reactor, slurries after ageing have the calcium hydroxide of a small amount of accumulation of salt in the surface soil, the carbonic acid gas input tube of past secondary carbonization tubular reactor feeds the carbon dioxide through volumetric concentration 〉=20% of purifying treatment, and itself and calcium hydroxide slurry are reacted.
Slurries after reacting in the secondary carbonization tubular reactor are directly led to calcium carbonate activation pond, and add tensio-active agent and handle, at last the slurries after the activation treatment are dehydrated processing, can obtain size distribution evenly, good dispersity, particle diameter be the nano-calcium carbonate about 30nm.
Adjusting calcium hydroxide mass concentration is 5%～10% calcium hydroxide slurry in the calcium hydroxide preparing pool, and deployed back is stored calcium hydroxide slurry in the calcium hydroxide slurry storage pool into.The temperature of the calcium hydroxide slurry in the calcium hydroxide slurry storage pool is controlled between 10 ℃～30 ℃, and to add the quality percentage composition account for the calcium hydroxide butt be 0.4% crystal formation directed agents magnesium chloride, sal epsom, a kind of in the water glass, add 0.2～2% dispersion agent sodium hexametaphosphate again, after the mixing and stirring, become to pump into calcium hydroxide slurry in the nuclear reactor toward a carbonization, and become the carbon dioxide that feeding has purified in the nuclear reactor toward a carbonization, the volumetric concentration of carbonic acid gas 〉=20%, the carbon dioxide of feeding with in the continuous contact reacts of slurries carburizing reagent Guan Zhongyu slurries.
Size by control flow of carbon dioxide gas amount is controlled speed of reaction, the water outer by slurries in the slurries carburizing reagent pipe and pipe carries out heat exchange, the control carbonization temperature is between 10 ℃～30 ℃, viscosity by slurries in the monitoring slurries carburizing reagent pipe changes, controlling a carbonization nucleation reacting slurry viscosity is 700mpa.s～850mpa.s, when monitor when the carbonization slurry viscosity of layer 700mpa.s～850mpa.s at present the slurries carburizing reagent pipe of one deck stop logical carbon dioxide.
Slurries after becoming the nuclear reactor internal reaction a carbonization are led to a carbonization grower, the temperature of time carbonization grower is controlled between 10 ℃～30 ℃, the carbon dioxide that feeds volumetric concentration 〉=20% of process purifying treatment carries out carbonization, make two ends unremitting slurries and the continuous contact reacts of carbon dioxide that repeats in the arched slurries carburizing reagent pipe continuously, reacted slurries flow out from the discharge pipe of a carbonization growth reactor bottom, resulting slurry pH value is 7～8, and particle diameter is about 80nm, size distribution is even, the nano-calcium carbonate slurries of good dispersity
The nano-calcium carbonate slurries that become the nuclear reactor internal reaction to obtain a carbonization lead to a carbonization ageing pond ageing and after 1～6 day slurries are extracted in the slurries carburizing reagent pipe of secondary carbonization tubular reactor, slurries after ageing have the calcium hydroxide of a small amount of accumulation of salt in the surface soil, the carbonic acid gas input tube of past secondary carbonization tubular reactor feeds the carbon dioxide through volumetric concentration 〉=20% of purifying treatment, and itself and calcium hydroxide slurry are reacted.
Slurries after reacting in the secondary carbonization tubular reactor are directly led to calcium carbonate activation pond, and add tensio-active agent and handle, at last the slurries after the activation treatment are dehydrated processing, can obtain size distribution evenly, good dispersity, particle diameter be the nano-calcium carbonate about 80nm.
Adjusting calcium hydroxide mass concentration is 5%～10% calcium hydroxide slurry in the calcium hydroxide preparing pool, and deployed back is stored calcium hydroxide slurry in the calcium hydroxide slurry storage pool into.The temperature of the calcium hydroxide slurry in the calcium hydroxide slurry storage pool is controlled between 20 ℃～40 ℃, and to add the quality percentage composition account for the calcium hydroxide butt be 0.3% crystal formation directed agents magnesium chloride, sal epsom, wherein a kind of of water glass and 0.2～2% dispersion agent sodium hexametaphosphate, after the mixing and stirring, become to pump into calcium hydroxide slurry in the nuclear reactor toward a carbonization, and become the carbon dioxide that feeding has purified in the nuclear reactor toward a carbonization, the volumetric concentration of carbonic acid gas 〉=20%, the carbon dioxide of feeding with in the continuous contact reacts of slurries carburizing reagent Guan Zhongyu slurries.
Size by control flow of carbon dioxide gas amount is controlled speed of reaction, the water outer by slurries in the slurries carburizing reagent pipe and pipe carries out heat exchange, the control carbonization temperature is between 32 ℃～33 ℃, viscosity by slurries in the monitoring slurries carburizing reagent pipe changes, controlling a carbonization nucleation reacting slurry viscosity is 600mpa.s～650mpa.s, when monitor when the carbonization slurry viscosity of layer 600mpa.s～650mpa.s at present the slurries carburizing reagent pipe of one deck stop logical carbon dioxide.
Slurries after becoming the nuclear reactor internal reaction a carbonization are led to a carbonization grower, the temperature of a carbonization grower is controlled between 31 ℃～35 ℃, the carbon dioxide that feeds volumetric concentration 〉=20% of process purifying treatment carries out carbonization, make two ends unremitting slurries and the continuous contact reacts of carbon dioxide that repeats in the arched slurries carburizing reagent pipe continuously, reacted slurries flow out from the discharge pipe of a carbonization growth reactor bottom, and resulting slurry pH value is
The footpath be nano-calcium carbonate slurries about 120nm, even, the good dispersity of size distribution
The nano-calcium carbonate slurries that become the nuclear reactor internal reaction to obtain a carbonization lead to a carbonization ageing pond ageing and after 1～6 day slurries are extracted in the slurries carburizing reagent pipe of secondary carbonization tubular reactor, slurries after ageing have the calcium hydroxide of a small amount of accumulation of salt in the surface soil, the carbonic acid gas input tube of past secondary carbonization tubular reactor feeds the carbon dioxide through volumetric concentration 〉=20% of purifying treatment, and itself and calcium hydroxide slurry are reacted.
Slurries after reacting in the secondary carbonization tubular reactor are directly led to calcium carbonate activation pond, and add tensio-active agent and handle, at last the slurries after the activation treatment are dehydrated processing, can obtain size distribution evenly, good dispersity, particle diameter be the nano-calcium carbonate about 120nm.
Embodiment 4
Adjusting calcium hydroxide mass concentration is 5%～10% calcium hydroxide slurry in the calcium hydroxide preparing pool, and deployed back is stored calcium hydroxide slurry in the calcium hydroxide slurry storage pool into.The temperature of the calcium hydroxide slurry in the calcium hydroxide slurry storage pool is controlled between 20 ℃～45 ℃, and to add the quality percentage composition account for the calcium hydroxide butt be 0.3% crystal formation directed agents magnesium chloride, sal epsom, wherein a kind of of water glass and 0.2% dispersion agent sodium hexametaphosphate, after the mixing and stirring, become to pump into calcium hydroxide slurry in the nuclear reactor toward a carbonization, and become the carbon dioxide that feeding has purified in the nuclear reactor toward a carbonization, the volumetric concentration of carbonic acid gas 〉=20%, the carbon dioxide of feeding with in the continuous contact reacts of slurries carburizing reagent Guan Zhongyu slurries.
Size by control flow of carbon dioxide gas amount is controlled speed of reaction, the water outer by slurries in the slurries carburizing reagent pipe and pipe carries out heat exchange, the control carbonization temperature is between 20 ℃～15 ℃, viscosity by slurries in the monitoring slurries carburizing reagent pipe changes, controlling a carbonization nucleation reacting slurry viscosity is 500mpa.s～600mpa.s, when monitor when the carbonization slurry viscosity of layer 500mpa.s～600mpa.s at present the slurries carburizing reagent pipe of one deck stop logical carbon dioxide.
Slurries after becoming the nuclear reactor internal reaction a carbonization are led to a carbonization grower, the temperature of a carbonization grower is controlled between 20 ℃～45 ℃, the carbon dioxide that feeds volumetric concentration 〉=20% of process purifying treatment carries out carbonization, make two ends unremitting slurries and the continuous contact reacts of carbon dioxide that repeats in the arched slurries carburizing reagent pipe continuously, reacted slurries flow out from the discharge pipe of a carbonization growth reactor bottom, resulting slurry pH value is 7～8, and particle diameter is about 200nm, size distribution is even, the nano-calcium carbonate slurries of good dispersity.
The nano-calcium carbonate slurries that become the nuclear reactor internal reaction to obtain a carbonization lead to a carbonization ageing pond ageing and after 1～6 day slurries are extracted in the slurries carburizing reagent pipe of secondary carbonization tubular reactor, slurries after ageing have the calcium hydroxide of a small amount of accumulation of salt in the surface soil, the carbonic acid gas input tube of living secondary carbonization tubular reactor feeds the carbon dioxide of volumetric concentration 〉=20% of process purifying treatment, and itself and calcium hydroxide slurry are reacted
Slurries after reacting in the secondary carbonization tubular reactor are directly led to calcium carbonate activation pond, and add tensio-active agent and handle, at last the slurries after the activation treatment are dehydrated processing, can obtain size distribution evenly, good dispersity, particle diameter be the nano-calcium carbonate about 200nm.
Claims (4)
1. carbonizer of producing nano-calcium carbonate, comprise calcium hydroxide preparing pool (4), the calcium hydroxide slurry storage pool (5) that is attached thereto, it is characterized in that: this carbonizer comprises that also an interconnective carbonization becomes nuclear reactor (1), a carbonization growth reactor (2), a carbonization ageing pond (6) successively, secondary carbonization tubular reactor (3) and calcium carbonate activation pond (7), a described carbonization becomes nuclear reactor (1) to be connected with the slurries output terminal of calcium hydroxide slurry storage pool (5);
A described carbonization becomes to be provided with slurries ingress pipe (8), slurries carburizing reagent pipe (9) and the discharge pipe (10) that from top to bottom connects successively in the nuclear reactor (1); The one end mouth of pipe of described slurries ingress pipe (8) extends to outside this reactor and is connected by the slurries output terminal of pipeline with calcium hydroxide slurry storage pool (5);
Be provided with the slurries ingress pipe (8), slurries carburizing reagent pipe (9) and the discharge pipe (10) that from top to bottom connect successively in the described carbonization growth reactor (2); The one end mouth of pipe of the slurries ingress pipe (8) of a described carbonization growth reactor (2) extends to outside this reactor and becomes the discharge pipe (10) of nuclear reactor (1) to be connected by pipeline and a carbonization, and the discharge pipe (10) of a described carbonization growth reactor (2) is connected by the slurries input terminus of pipeline with a carbonization ageing pond (6);
Be provided with slurries carburizing reagent pipe (9) in the described secondary carbonization tubular reactor (3), the mouth of pipe of these slurries carburizing reagent pipe (9) one ends extends to outside this reactor and is connected by the slurries output terminal of pipeline with a carbonization ageing pond (6), and the another port is stretched out in this reactor bottom and is connected in the calcium carbonate activation pond (7).
2. the carbonizer of production nano-calcium carbonate according to claim 1, it is characterized in that: a described carbonization becomes in the interior slurries carburizing reagent pipe (9) of nuclear reactor (1), a carbonization growth reactor (2) and secondary carbonization tubular reactor (3) to be provided with carbonic acid gas porous reaction pipe (12), and this carbonic acid gas porous reaction pipe (12) is communicated with the carbonic acid gas input tube (11) that is arranged at the interior side of this reactor.
3. the carbonizer of production nano-calcium carbonate according to claim 2 is characterized in that: a described carbonization becomes the carbonic acid gas porous reaction pipe (12) in nuclear reactor (1), a carbonization growth reactor (2) and the secondary carbonization tubular reactor (3) to be provided be used to making the catalytic hole of carbonic acid gas and slurries; Slurries ingress pipe (8) in each reactor is the continuous unremitting repetition bow-shaped structural in two ends with slurries carburizing reagent pipe (9) and carbonic acid gas porous reaction pipe (12), and the bore of discharge pipe (10) is 2 times of bore of slurries carburizing reagent pipe (9).
4. one kind is utilized the method that each described carbonizer is produced nano-calcium carbonate among the claim 1-3, and its step is as follows:
1) modulation of calcium hydroxide slurry:
The concentration of deployed calcium hydroxide slurry in the calcium hydroxide preparing pool, and in calcium hydroxide slurry, add crystal formation directed agents and dispersion agent sodium hexametaphosphate, and mixing and stirring;
2) storage of calcium hydroxide slurry:
Will be in the calcium hydroxide preparing pool deployed slurries be extracted in the calcium hydroxide slurry storage pool and store;
3) carbonization nucleation reaction treatment:
Slurries in the calcium hydroxide slurry storage pool are led to a carbonization become slurries ingress pipe in the nuclear reactor, and become carbonic acid gas input tube in the nuclear reactor to feed carbon dioxide through purifying treatment toward a carbonization, make slurries and carbon dioxide contact reacts in slurries carburizing reagent pipe, obtain calcium hydroxide and calcium carbonate mixing suspension, reacted slurries are discharged from the discharge pipe in this reactor;
4) a carbonization growth response is handled:
The reacted slurries of carbonization nucleation are led to the slurries ingress pipe in the carbonization growth reactor one time, and the carbonic acid gas input tube in carbonization growth reactor feeds the carbon dioxide through purifying treatment, make calcium hydroxide and carbon dioxide contact reacts in slurries carburizing reagent pipe in the slurries, obtain the nano-calcium carbonate slurries, reacted slurries are discharged from the discharge pipe of this reactor;
5) ageing is handled:
Slurries after the carbonization growth response are led in a carbonization ageing pond carry out ageing, remove the impurity in the nano-calcium carbonate slurries and make the particle diameter of nano-calcium carbonate even;
6) the secondary carburizing reagent is handled:
Slurries after ageing is handled have the calcium hydroxide of a small amount of accumulation of salt in the surface soil, slurries after a carbonization ageing pond ageing are extracted into the slurries carburizing reagent pipe of secondary carbonization tubular reactor, and the carbonic acid gas input tube in carbonization growth reactor feeds the carbon dioxide through purifying treatment, makes calcium hydroxide and carbon dioxide contact reacts in slurries carburizing reagent pipe in the slurries;
7) activation treatment:
To in secondary carbonization tubular reactor, lead to calcium carbonate activation pond by reacted nano-calcium carbonate slurries, and add tensio-active agent and handle;
8) dehydrate processing:
Slurries after the pond activation dewater with activating at calcium carbonate, drying treatment, obtain required nano-calcium carbonate calcium product;
In the described step 1), the mass concentration of the calcium hydroxide slurry of described allotment is 5%～15%; Described crystal formation directed agents is a kind of in magnesium chloride, sal epsom, the water glass, the crystal formation directed agents of adding and the quality of dispersion agent sodium hexametaphosphate be calcium hydroxide butt in the calcium hydroxide slurry the quality percentage composition 0.1%～2%;
In described step 3), step 4) and the step 6), the carbon dioxide that feeds in each carburizing reagent is the carbon dioxide of volumetric concentration 〉=20%;
In described step 3), step 4) and the step 6), carry out heat exchange by the outer water of the slurries in the slurries carburizing reagent pipe and pipe in each carburizing reagent, make the carbonization temperature control of each carburizing reagent between 10～45 ℃.
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| CN104016391A (en) * | 2014-04-10 | 2014-09-03 | 连州市凯恩斯纳米材料有限公司 | Method for preparing nanometer calcium carbonate for organic silicone electronic sealant by adopting continuous carbonization device |
| CN104843757B (en) * | 2015-04-16 | 2017-01-04 | 四川海雅粉体科技有限责任公司 | A kind of coiled nano-calcium carbonate carbonization system |
| CN106345265B (en) * | 2016-08-26 | 2019-02-05 | 华北电力大学 | Integrate the coal fired power plant system of secondary carbonisation calcium oxide circulation decarbonization system |
| CN109180214A (en) * | 2018-09-27 | 2019-01-11 | 佛山齐安建筑科技有限公司 | A kind of calcium carbonate thermal insulation material and preparation method thereof |
| CA3168044A1 (en) | 2020-02-25 | 2021-09-02 | Michael Joseph Weiss | Methods and systems for treatment of limestone to form vaterite |
| US11377363B2 (en) | 2020-06-30 | 2022-07-05 | Arelac, Inc. | Methods and systems for forming vaterite from calcined limestone using electric kiln |
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| CN1749168A (en) * | 2005-10-21 | 2006-03-22 | 颜鑫 | Continuous bubbling carbonizing new process for producing super fine active calcium carbonate |
| CN101525147A (en) * | 2008-12-04 | 2009-09-09 | 兰州理工大学 | Preparation method of nano calcium carbonate |
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