CN1040739C - Precipitated calcium carbonate preparation using waste from dicyandiamide plant - Google Patents
Precipitated calcium carbonate preparation using waste from dicyandiamide plant Download PDFInfo
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- CN1040739C CN1040739C CN93117020A CN93117020A CN1040739C CN 1040739 C CN1040739 C CN 1040739C CN 93117020 A CN93117020 A CN 93117020A CN 93117020 A CN93117020 A CN 93117020A CN 1040739 C CN1040739 C CN 1040739C
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- calcium carbonate
- light calcium
- dicyandiamide
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Abstract
The present invention relates to an utilization method of industrial waste slag of dicyandiamide. On the basis that impurities, such as water, river sands, organic substances containing nitrogen, etc., are removed from industrial waste slag of dicyandiamide to prepare light calcium carbonate containing carbon with the technique methods of natural or mechanical dewatering, high-temperature baking, winnowing, sieving, etc., free carbon ingredients are further separated from the light calcium carbonate with a combustion decarbonizing method, and the light calcium carbonate is purified into light calcium carbonate chemical products with high purity. The quality and the performance are completely equivalent to those of light calcium carbonate produced with the traditional technique by using limestone as raw materials, and the light calcium carbonate with high purity can be used as filling agents widely applied to the production of light industry products, such as rubber, plastic, paint, paper, decorative heat-insulating materials, etc. The present invention obtains the satisfactory use effect, and accordingly the application range and the use value of the light calcium carbonate are greatly increased.
Description
The present invention is a kind of processing method of chemical industry waste residue, is that improved a kind of new technology method and product are carried out in invention to existing number of patent application 91109467.9 " utilizing dicyandiamide industry waste residue to produce filler of high molecular synthetic products ". Namely utilize harmful waste residue of discharging in the production of chemical products dicyandiamide to process processing for raw material, purify and make lightweight calcium carbonate producing on the basis that contains carbon lightweight calcium carbonate further processing. Thereby obtain, enlarge the effect of product range of application and raising product use value.
In chemical products dicyandiamide production process, discharge a kind of waste residue, quantity is very large, one ton of finished product of every production goes out the quantity of slag and reaches about 12 tons, process such as the passive method of stacking with expropriation of land, not only waste soil resource and blowdown funds, and wherein nitrogenous organic matter flows into the lake,pool and well storehouse and will stain water quality, becomes public hazards. Existing " utilizing dicyandiamide industry waste residue to produce filler of high molecular synthetic products " invention; that this kind waste residue is removed harmful composition and impurity; change a kind of chemical industry material by winnofil and graphite mould carbon composition into; can replace pure white light calcium and make filler; to eliminating this public hazards, protection of the environment has been walked out a gratifying step. But the final product that this technology is produced " contains carbon lightweight calcium carbonate ", because failing that the free carbon element that contains in the material composition is separated, make its outward appearance gray, can only be at dark colour rubber, use as filler in the Polymer Synthesizing goods such as plastics, greatly limited range of application and the use value of its product.
The objective of the invention is and to do further in-depth processing utilizing dicyandiamide industry waste residue to produce the basis that contains carbon lightweight calcium carbonate, contained free carbon element composition all takes off and removes in a kind of new process means its material being formed, make its winnofil of finally making pure matter (lightweight), become the filler chemical products of broad spectrum type, the industry such as rubber, plastics, papermaking, coating, decorative heat preservation material that can be widely applicable for any color is made raw materials for production, thereby improve widely range of application and the use value of product, given play to larger Social benefit and economic benefit.
The objective of the invention is to carry out like this:
One, technological principle
The waste residue of discharging in the filter tank is crossed by factory in dicyandiamide production, the danger is contained outside the large quantity of moisture (up to 48～52%), the heavy calcium carbonate microparticle (accounting for 29～37%) that system is generated by lime nitrogen hydrolysis liquid carbonization decalcification, lime is worn the free carbon element particulate (accounting for 3.3～5.2%) of carrying secretly in the raw material, and sand filtration is reclaimed a small amount of dicyandiamide residual in the coarse granule river sand (accounting for 9～13%) that stays behind the mother liquor and the filtering mother liquor not, urea etc. and contained nitrogen organic (accounting for 0.6～1.4%) etc. and become to be grouped into (the former slag material of the wet row component law that is depicted as recent sampling analysis measuring such as accompanying drawing one).
Form according to above-mentioned substance, the series of process means such as existing " utilize dicyandiamide industry waste residue produce filler of high molecular synthetic products " technology method adopts that nature or mechanical dehydration, high temperature baking are burnt, screening or selection by winnowing, separated and take off except contained moisture, river sand in the material of slagging tap, contain the class impurity such as nitrogen organic, when keeping the main active ingredient of winnofil, still retain the difficult free carbon element composition that separates. The free carbon element of this kind is a kind of without typing carbon, easy firing, can utilize the difference of its ignition temperature and Decomposition of Calcium Carbonate temperature, material placed above carbon particulate burning-point (650-700 ℃) be lower than in the temperature scope of Decomposition of Calcium Carbonate temperature (825～850 ℃), its spontaneous combustion, oxidation, volatilization are taken off except (being depicted as free carbon element combustibility rule such as accompanying drawing two; Accompanying drawing three is depicted as free carbon element burning temperature controlling range rule) winnofil that obtains at last, its purity is more than 99%, except because the difficult molten element of trace exists products appearance color (whiteness) being subject to some impacts, every quality index all surpasses or near the technical indicator (being depicted as preproduction by the measured result of national standard method check such as accompanying drawing five) that " winnofil (lightweight) standard GB/T 4794-84 " stipulates, can satisfy the industries such as rubber, plastics, papermaking, coating, decorative heat preservation material to technology requirement and the quality standard of filler.
Two, technological process
According to above-mentioned technological principle, for dicyandiamide sludge as material being transformed into high-quality lightweight calcium carbonate chemical products, can take a series of physics to process processing with process chemistry, its technological process of production design is as follows:
1. dewater, take from the slag material of dicyandiamide production factory pollution discharge pond, be the underflow shape, water content is very large, must take first the place to stack nature dehydration or enforcement plant equipment powerful dehydration, with the near minimum degree of its water content, convenient and energy savings creates conditions for the following process procedure operation.
2. primary election: produce lumps because being mingled with the bulky grain foreign material in the raw material waste residue and naturally boning, should adopt as the type equipment such as rolling roll cylinder are smashed material and the primary election removal of impurities.
3. oven dry: the slag material after dehydration and primary election is half dry powder-shaped, drops into oven dry equipment, with the evaporation of the moisture in the material, makes its drying.
4. calcination: the material after will drying drops into high-temperature heating device, the temperature that strict control is suitable, make the abundant spontaneous combustion oxidation volatilization of free carbon element particulate wherein in stirring and flowing, contain nitrogen organic and also decompose simultaneously volatilization, the mist of generation enters the high-altitude from flue.
5. sieve or selection by winnowing: the material behind high temperature sintering has been winnofil, wherein still is mixed with part coarse granule river sand, and it is dropped into screening machine or winnowing machine, and coarse granule impurity is separated with calcium carbonate microparticle.
6. packing: remove the white fine powder that obtains behind the coarse granule impurity and be final product through screening or selection by winnowing, can pack at screening machine or the little powder discharging opening of winnowing machine, after quality inspection is qualified, dispatch from the factory.
(be depicted as dicyandiamide sludge as material such as accompanying drawing four and produce the test record of winnofil overall process technological experiment)
Three, quality inspection and technical standard
Take dicyandiamide sludge as material as raw material, winnofil by above-mentioned technological process production, with regard to the chemical reaction process that its material generates, through-stone ash nitrogen hydrolysis generation calcium hydroxide adds carbon dioxide chemical combination and forms, with become quick lime to be dissolved in water to generate calcium hydroxide to add the traditional handicraft that carbon dioxide chemical combination forms be in full accord with the lime stone calcination, the physico-chemical property of its product and traditional handicraft product are also without any difference. For this reason, in quality inspection and management, also should unanimously with traditional product adopt technical standard and the method for inspection of standard GB/T 4794-84, but because this product system produces take dicyandiamide sludge as material as raw material, the overall process that it is purified to processing from the reactant to the product, experienced the production link of lime nitrogen and two different products of dicyandiamide, in succession infiltrated multiple external material, though got rid of harmful composition and impurity through the series of process method as far as possible, but be difficult to avoid the existence of minimal residue thing, thereby cause " sour insoluble matter " index number to transfinite and the gap (shown in accompanying drawing one, accompanying drawing five) of " whiteness " index, therefore, in quality inspection and management, need again according to actual conditions the technical indicator of GB regulation to be made other revision. (shown in accompanying drawing six, being this technical target of the product according to winnofil (lightweight) GB GB4794-84 establishment) can be used as the foundation of manufacturing enterprise's drawing up the enterprise standard and implementation quality management.
Four, secondary pollution situation
From above-mentioned technological process as can be known, dicyandiamide sludge as material according to present technique processing processing, wherein unique harmful composition is to contain on a small quantity nitrogen organic (mainly being residual dicyandiamide), though must at high temperature decompose chemical combination ammonification or nitrogen oxide gas discharges, but content seldom, can not cause environmental pollution, as calculating with the saturated output of per hour processing 2 tons in waste residue, wherein contain the cyanogen organic matter and count 20 kilograms with the highest content 1%, be converted into the larger chlorine dioxide discharge capacity of harm by molecular weight and be about 11 kilograms, (" the tentative standard GBJ4-73 of industry " three wastes " discharging " regulation nitrogen oxide is converted into NO as long as liftoff 20 meters of air flue emission mouth, its discharge capacity can not exceed national pollution control standard2The discharging limit be that 20 meters of chimney height allow 12 kg/hours of discharge capacitys). Such as slag material isolated coarse granule river sand in screening or selection by winnowing process, building trade can be all supplied with as the first-class sand material use of concrete and masonry mortar in addition, more secondary pollution can be do not caused.
Dicyandiamide industry waste residue material forms test record
Accompanying drawing one
| Specimen coding | The wet former slag specimen product tests of row (g) | Sample test (g) after the oven dry screening | Be converted into each component content (%) of the former slag of wet row | |||||||||||
| Samples weighing | 100 ℃ of bakings were weighed in 2 hours | 200 order inch is weighed later | Samples weighing | 300 ℃ of calcinations were weighed in 2 hours | Excessive HoL reaction post-drying | Consider 850 ℃ of calcinations of slag weighed in 2 hours | Moisture | River sand | Contain nitrogen organic | Winnofil | Free carbon element | Trace impurity | ||
| The filter paper dry weight | Filter residue filter paper dry weight | |||||||||||||
| 1 2 3 4 5 6 7 8 9 10 | 100 100 100 100 100 100 100 100 100 100 | 48 50 48 49 51 47 48 48 52 51 | 10.4 9.9 11.3 10.7 9.8 13.3 10.8 11.7 9.3 10.9 | 1.0006 1.0041 1.0033 0.9981 1.0071 0.9977 1.0029 1.0001 0.9956 1.0055 | 0.9843 0.9804 0.9867 0.9791 0.9727 0.9850 0.9767 0.9812 0.9799 0.9848 | 0.8027 0.7983 0.8090 0.8044 0.8111 0.8071 0.8101 0.7956 0.8063 0.8099 | 0.9385 0.9183 0.9388 0.9554 0.9186 0.9331 0.9035 0.9401 0.9228 0.9470 | 0.0057 0.0039 0.0027 0.0041 0.0030 0.0036 0.0052 0.0044 0.0039 0.0046 | 52 50 52 51 49 53 62 52 48 49 | 10.4 9.9 11.3 10.7 9.8 13.3 10.8 11.7 9.3 10.9 | 0.61 0.95 0.61 0.60 1.40 0.43 0.97 0.69 0.67 0.82 | 31.91 34.35 31.34 31.91 35.40 29.01 32.77 30.37 37.04 33.81 | 4.89 4.64 4.66 5.54 4.28 4.13 3.27 5.08 4.83 5.28 | 0.21 0.16 0.10 0.16 0.12 0.15 0.19 0.16 0.17 0.18 |
| The mensuration program | Moisture | River sand | Contain nitrogen organic | Winnofil | Free carbon element trace impurity | 48 ～ 52 | 9 ～ 13 | 0.6 ～ 1.4 | 29 ～ 37 | 3.3 ～ 5.5 | 0.10 ～ 0.21 | |||
Free carbon element combustibility is surveyed sincere record in accompanying drawing two dicyandiamide sludge as material
Accompanying drawing three
| Sample source | The former slag of wet row decomposes calcium carbonate with excessive hydrochloric acid, stays water washing to filter with steaming, and removes coarse granule river sand, makes free carbon dust sample with 200 orders/inch sieve sieve after the filter residue oven dry | Method of testing | Take by weighing sample 1 gram, in 600～800 ℃ of scopes, with different temperatures calcination 30 minutes, measure its volatilization part, as can be known burning degree of free carbon element. | |||||||
| The sample sequence number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Samples weighing (g) | 1.0013 | 1.0078 | 1.0045 | 0.9981 | 1.0020 | 0.9956 | 1.5054 | 1.0007 | 0.9992 | 1.0023 |
| The burning temperature (℃) | 600 | 520 | 640 | 560 | 680 | 700 | 720 | 740 | 760 | 800 |
| (g) weighs after the burning | 1.0012 | 1.0070 | 0.9253 | 0.1852 | 0.0626 | 0.0180 | 0.0043 | 0.0046 | 0.0044 | 0.0048 |
| Volatilization minute calculating (%) | 0 | 0 | 7.88 | 81.44 | 93.75 | 98.19 | 99.57 | 99.54 | 99.56 | 99.52 |
Contain free carbon element in the carbon lightweight calcium carbonate, the burning method is taken off except the temperature controlling range test record
| Sample source | The former slag of wet row burns in 300 ℃ of lower fully bakings, takes off except moisture and contains nitrogen organic, screens out coarse granule river sand with 200 orders/inch, makes to contain carbon lightweight calcium carbonate sample. | Method of testing | Take by weighing sample 1 gram, the different temperatures calcination is 30 minutes in 600～850 ℃ of scopes, and its residue is decided calcium oxide, calcium carbonate content with capacity check respectively, measures free carbon content with the weight method, can find out the optimum temperature range of purification calcium carbonate. | |||||||
| The sample sequence number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Samples weighing (g) | 0.9991 | 1.0017 | 1.0069 | 1.0033 | 0.9965 | 1.0004 | 1.0051 | 0.9978 | 1.0015 | 1.0026 |
| The calcination temperature (℃) | 600 | 650 | 700 | 720 | 740 | 760 | 780 | 800 | 820 | 850 |
| Calcium oxide content (%) | 0.064 | 0.059 | 0.061 | 0.067 | 0.063 | 0.058 | 0.168 | 13.94 | 43.08 | 50.46 |
| Calcium carbonate content (%) | 90.43 | 90.67 | 90.41 | 90.36 | 90.39 | 90.41 | 90.28 | 66.48 | 14.62 | 1.05 |
| Free carbon content (%) | 8.97 | 1.63 | 0.016 | 0。003 | 0 | 0 | 0 | 0 | 0 | 0 |
Accompanying drawing four
Dicyandiamide sludge as material is produced calcium carbonate overall process observation test record
| Temperature is burnt in baking | The baking burning time | Weighing after baking is burnt | Phenomenon was described after baking was burnt | Remarks |
| Room temperature | Original sample | 3kg | The former slag of wet row is deposited partial dehydration in March | Naturally former slag dewaters |
| 100℃ | 2 hours | 1.9050kg | Be weighed as .48700 after sieving with 200 orders/inch | Contain the not yet denitrogenation of carbon calcium |
| 700℃ | 0.5 hour | 1.4459kg | The top layer sample bleaches, and internal layer still stirs even rear color for grey and slightly shoals | The spontaneous combustion of the denitrogenation part of having dewatered carbon element. |
| 700℃ | 1 hour | 1.3891Kg | Sample is most of to be become certainly, still has the part grey to stir even rear color and further shoals | The spontaneous combustion of most of carbon element |
| 700℃ | 1.6 hour | 1.3222kg | Sample becomes certainly substantially | Spontaneous combustion is incomplete for residual few carbon element |
| 700℃ | 2 hours | 1.3184kg | Sample all bleaches, and it is slightly poorer than traditional handicraft production calcium carbonate certainly to spend | Carbon element all volatilizees, and makes calcium carbonate |
| Test method is taken a sample from former slag is dewatered in the waste residue stockyard naturally, and moisture is removed in first oven dry, sieve removes coarse granule river sand again, then place in the resistance furnace, select best calcination temperature, observe every half an hour and weigh once until till sample all makes pure calcium carbonate. | ||||
Accompanying drawing five
Dicyandiamide sludge as material is produced lightweight calcium carbonate preproduction quality index detection record
| Test item | Calcium carbonate content (%) | Moisture (%) | Residue on sieve (%) | Settling volume (ml/g) | Hydrochloric acid insoluble substance (%) | Free alkali (in Cao %) | Iron (%) | Manganese (%) | Whiteness (%) | |
| 125/um | 45/um | |||||||||
| Heavy heavy stone used as an anchor calcium carbonate (lightweight) GB GB4794-84 | ≥0.8 | ≤0.3 | ≤0.005 | ≤0.5 | ≥2.8 | ≤0.1 | ≤0.1 | ≤0.1 | ≤0.0045 | ＞80 |
| Dicyandiamide sludge as material is produced the winnofil measured result | 99.35 | 0.09 | Nothing | 0.29 | 2.9 | 0.43 | 0.071 | 0.028 | 0.0012 | 60 |
| The contrast conclusion | Can standard up to standard | Can standard up to standard | Can standard up to standard | Can standard up to standard | Can standard up to standard | Near standard | Can standard up to standard | Can standard up to standard | Can standard up to standard | Certain gap is arranged |
Accompanying drawing six
Dicyandiamide sludge as material is produced the technical indicator of light calcium carbonate product and is drawn up a plan for
| Technical indicator | Calcium carbonate content (%) | Moisture (%) | Residue on sieve (%) | Settling volume (ml/g) | Hydrochloric acid insoluble substance (%) | Free alkali (in cao %) | Iron (%) | Manganese (%) | Whiteness (%) | |
| 125/um | 45/um | |||||||||
| Winnofil (lightweight) GB GB4794-84 | ≥98 | ≤0.3 | ≤0005 | ≤0.5 | ≥2.8 | ≤0.1 | ≤0.1 | ≤0.1 | ≤0.0045 | ＞80 |
| Dicyandiamide sludge as material is produced the winnofil company standard | ≥98 | ≤0.3 | ≤0.005 | ≤0.5 | ≥2.8 | ≤0.5 | ≤0.1 | ≤0.1 | ≤0.0045 | ＞60 |
Claims (1)
1. method of utilizing dicyandiamide industry waste residue to produce lightweight calcium carbonate, after it is characterized in that using nature drying or mechanical dehydration, utilize free carbon element ignition temperature (700 ℃ of 650-) contained in this waste residue and the difference between the Decomposition of Calcium Carbonate temperature (825-850 ℃), be placed on the interior calcination of temperature scope that surpasses the carbon burning-point and be lower than the divided calcium carbonate solution point, make wherein contained carbon particulate nature, oxidation, volatilization is taken off removes, also volatilization is taken off except containing nitrogen organic simultaneously, and then remove river sand with selection by winnowing or screening method, make moisture contained in this waste residue, river sand, contain nitrogen organic, all dirt such as free carbon element separated, reach the last purification of active ingredient winnofil, thereby produce lightweight calcium carbonate chemical products.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93117020A CN1040739C (en) | 1993-09-08 | 1993-09-08 | Precipitated calcium carbonate preparation using waste from dicyandiamide plant |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93117020A CN1040739C (en) | 1993-09-08 | 1993-09-08 | Precipitated calcium carbonate preparation using waste from dicyandiamide plant |
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| Publication Number | Publication Date |
|---|---|
| CN1100067A CN1100067A (en) | 1995-03-15 |
| CN1040739C true CN1040739C (en) | 1998-11-18 |
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| CN93117020A Expired - Fee Related CN1040739C (en) | 1993-09-08 | 1993-09-08 | Precipitated calcium carbonate preparation using waste from dicyandiamide plant |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106012012B (en) * | 2016-05-31 | 2018-10-23 | 宁夏大学 | The method for preparing calcium carbonate crystal whisker with dicyandiamide sludge as material |
| CN109319781B (en) * | 2018-09-12 | 2020-05-29 | 浙江工业大学 | Method for preparing coal-based hierarchical pore activated carbon material by using cyanamide waste residues as template |
| CN110776265A (en) * | 2019-10-15 | 2020-02-11 | 宁夏贝利特生物科技有限公司 | Method for preparing lime by utilizing cyanamide black slag for pelletizing |
| CN114773776A (en) * | 2022-05-06 | 2022-07-22 | 安徽银隆塑业科技有限公司 | Halogen-free flame-retardant polyformaldehyde granules and production process thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1071181A (en) * | 1991-09-24 | 1993-04-21 | 屠志康 | Utilize the Dyhard RU 100 industrial residue to produce filler of high molecular synthetic products |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1071181A (en) * | 1991-09-24 | 1993-04-21 | 屠志康 | Utilize the Dyhard RU 100 industrial residue to produce filler of high molecular synthetic products |
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