SU1623999A1 - Method for producing carbon black - Google Patents

Abstract

The introduction of soot to the technology of soot production using the kiln method used in polymer compositions, for example in rubber, makes it possible to increase the specific external surface and the structure of the soot, reduce its roughness and depend on the strength of the rubber when soot is filled. The hydrocarbon feedstock is thermally decomposed in the combustion products of fuel with the formation of carbon black products at 1450-1300 ° C, expanding the flow of the latter and then introducing alkali metal compounds in the amount of 25-95Z from 800 to 1400 ° C. the quantities, the rest of these compounds are introduced into the soot gas products while they are cooled with water at 200-750 ° C before the soot is separated, and the total amount of the compounds introduced is 0.005-0.500% by weight of the raw material. Soot properties: specific surface, m / g: geometric 98-100 adsorption (in phenol) 112-1175 ext. 106-117; absorptive (for nitrogen) 113-119, iodine number 110-117 mg / g, absorption of dibutyl fluoride 108-111 ml / 100 g of carbon black, pH of the aqueous suspension 7.6-8.0, delicacy 0.20-0.23 % Rubber performance: stress at 300% elongation of 148–159 kgf / cm2; tearing strength: 307–327 kgf / cm2. 2 hp F-chy, 1 ill., 1 tab. § (L

Description

The image refers to the production of an obedient macherpanov, namely, to the furnace production by furnace method, spon h. smog in polymer

COMPOSITIONS.

In the drawing, it is an implementation implementation (manual for iv- (nr i / k and reactor for eio ocvne.1. IB (Ench, longitudinal section).

Reactor, m iio.:v4v-nn4 with a breeze includes mills MMiHi le with oo p. P iioi. gedova- hemno a4i pv I r -r hhch diamem 220 mm and g-ui and, m i di. mp ran -

Generic burners 2, see the folding nozzle 3 with a diameter of mm and a length of 3300 mm. At a distance of 200 mm from the inlet highlander nozzle 5, radial nozzles for feeding the raw material are installed opposite each other, at a distance of 200 mm from the output highlander of the nozzle 3 in its side wall a channel 0 is made for measuring –perme, and at a distance of 500, 1000 , 2500 and 3000 mm from the input of the TOJMM and Achera 4 reactions to its combatants and channels I, II, III and 1 and I IH pi, my INS

with

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chn in the reactor material flows. The reactor communicates with the reaction product supply circuit successively to a heat exchanger-heat exchanger 5, a cooler-irrigator 6, cyclones 7 for pre-separation of soot and bag filters 8 for the final separation of soot from the gaseous products.

Example 1. 200 m3 / h of natural gas and 2300 m3 / h of air with a pressure of 0.5 kg / / cm2 and a temperature of 200 ° C are fed into the combustion chamber 1 through tangential burners 2. The temperature of the products formed during their combustion at the entrance to the nozzle 3 is 1520 C. Using raw nozzles, 700 kg / h of hydrocarbon feed is injected into nozzle 3 at 250 ° C with a correlation index of 115, density of 1.036 g / cm3, viscosity at 50 ° C 5.2 cSt, alkalinity of 0.012 mg / l. The soot-eae products formed as a result of the thermal decomposition of raw materials enter the chamber 4, where their flow expands. An aqueous solution of sodium hydroxide with a concentration of 0.33 wt.% In an amount of 35 g / g is fed to channel I of chamber 4, which corresponds to O, 1 2 KG / sodium hydroxide or 0.017% for raw materials (68% of the total amount of sodium hydroxide) . Through channel III, water is supplied to chamber 4 by means of a mechanical nozzle for pre-cooling of carbon black products. The water flow is limited by the set temperature of 1100 ° C, measured with a pyrometer installed in channel III. Channel IV is fitted with a mechanical nozzle through which water with sodium hydroxide in the amount of 0.057 kg / h is supplied to chamber 4, which is 0.003% of the feedstock or 32% of the total amount of sodium hydroxide. The total amount of alkali metal compound is 0.025% by weight of the raw material. The amount of water leaving chamber 4 is limited by a given temperature of 600 ° C. Next, the carbon black products are cooled in the heat exchanger-heat exchanger 5 and the cooler-irrigator 6. After cooling, the soot is separated from the gaseous products in cyclones 7 and filter 8, compacted in a compactor, granulated with a wet method, dried in a drying drum and packed.

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The data on the properties of carbon black and the rubber obtained from it are given in the table (experiment 5).

Example 2. The conditions of example 1 (run 5) are repeated, but the temperature of the precooling of soot-eae products is changed (runs 6-10).

Example 3. Experimental conditions 5 are repeated, but with the additional addition of sodium hydroxide, the temperature of the carbon black products is changed (tests 11-16).

Example 4. Experimental conditions 5 were repeated, but the total amount of sodium hydroxide changed (experiments 17-22).

Example 5. Experimental conditions 5 were repeated, but the amount of sodium hydroxide additionally changed (experiments 23-28).

Example 6. Experimental conditions 5 are repeated, but various alkali metal compounds are used: potassium hydroxide (KOH) - experience 29, potassium nitrate (KNO) - experience 30, potassium carbonate (KaC03) - experience 31, sodium nitrate NaNOj - experience 32 .

Example 7 (known) Through a tangential burner 2, 200 m3 / h of natural gas and 2300 m3 / h of air with a pressure of 0.5 kg / cm2 and a temperature of 200 ° C are fed into the combustion chamber 1. The temperature of the combustion product formed is 1520 ° C. Using raw nozzles, 700 kg / h of hydrocarbon feed is injected into the nozzle 3 at 250 ° C with a correlation index of 115, a density of 1.036 g / cm3, a viscosity at 50 ° C of 5.2 cSt, an alkalinity of 0.012 mg / l. Sodium hydroxide is fed into the carbon dioxide products in the amount of 0.177 kg / h, which corresponds to 0.025% of the amount of the raw material, the flow is expanded, the soot-gas product is aged (path of carbon black products after expansion of 3000 mm to channel 4), through channel IV Using a mechanical nozzle, the carbon black products are cooled with water up to 600 ° C, then the cooling is continued, filtered, compacted, granulated and the carbon black is dried according to Example 1 (experiment 1).

The conditions of the experiment are repeated, changing the total amount of sodium hydroxide (experiments 2-4).

Data on the release of carbon black and its physico-chemical characteristics are given in the table.

The resulting soot samples were tested as filler in standard rubber mixtures based on synthetic rubber SKMS-30 DRK, wt.h.

Rubber SKMS-30 ARK100

Stearin5

Zinc Oxide5

Altax2

Sulfur2

Soot50

The mixture is vulcanized with 2-millimeter plates and the conditioned stress is determined at 300% elongation, and the conventional stress is determined at break.

The data on the properties of the obtained win ses are given in the table.

How should h-; | Tablets' data with an optimal total amount of octins of an alkali metal compound is 0.005-0.50% of the raw material, (experiment 5, 18, 19, 20 and 21) The use of an alkali metal compound in quantities below 0.005 l results in soot not different from the soot obtained by a known method (experiment 17, 1-4) An increase in the total amount of alkali metal above 0.500% leads to an increase in the pH of the soot suspension, ash content, a decrease in rubber values (experiment 22). X-ray analysis of the carbon black shows a sharp uve There is a coherent dispersion area, i.e. a reduction in the ordering of the microstructure of the soot particle to a certain quantitative limit of the alkali metal (in this case, the amount of sodium hydroxide is 0.5%).

The optimal amount of additionally introduced compounds of small metals into soot products is that when they are cooled, the PHPCHCH 5-75% of the total number of compounds (experiments 24-27). The introduction of a surplus below 5% of the total amount of alkali metal compounds leads to a decrease in the quality indicators of carbon black and rubber based (experiment 23) An increase in the amount of additional injected gas, t ;: RHPPS 75% of the total amount of soot leads to soot not different from the known (experiment 29),

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The optimum temperature for the pre-cooling of the carbon black products after the introduction of alkali metal compounds is 600-1400 ° C (experiments 5, 7-9).

For this temperature range, an extreme value of the endothermic reaction of the interaction of carbon black with alkali metal compounds is characteristic. Adding at this time to the carbon black products of alkali metal compounds does not cause them to be disfused. soot surface and the extermination of endothermic reactions. At temperatures above 1400 ° C, the carbon black does not differ in its properties from the known (OID-IT 6). A decrease in temperature below 800 ° C also does not improve the properties of carbon black (OPMT 10).

From the experimental data listed in the table, it also follows that the additional introduction of alkali metal compounds with further cooling of gas products also leads to a positive result (experiments 12-15). For this temperature range, an exothermic reaction of the interaction of carbon black with alkali metal compounds is characteristic. At temperatures below 200 ° C and above 750 ° C, the exothermic reaction of the compounds in the ririx gap does not occur with soot and does not differ from the well-known properties (experiments 11 and 16).

The effect of other alkali metal compounds IB HI metal properties and carbon black yield is similar to the effect of sodium hydroxide (experiments 29-32).

In this way, the proposed method for producing soot reduces the amount of soot roughness, makes it smoother, improves the external and reduces the adsorption surface, improves the structure of soot, as well as enhances its properties by 12-15% in strength and 10-12%. module.

Claims (3)

1. A method of producing carbon black, including burning fuel with air, supplying hydrocarbon raw materials to the combustion products of fuel, thermal decomposition of hydrocarbon raw materials with the formation of carbon black products with a temperature of 1450-1800 C, introduction into the carbon black products of alkali metal compounds, expanding the flow of carbon black gas products with subsequent cooling and separation of carbon black from them, characterized in that, in order to increase the specific external surface and structure of the carbon black, reduce its roughness and increase 200-750 ° C. Additional alkali metal compounds are added in the amount of 5-75% of the total amount of alkali metal compounds administered. 2. The method according to claim 1, characterized in that the total number of metal compounds is a composition of rubber strength during filling 10 liters of 0.005-0.500% by weight of raw materials, carbon black, alkali metal compounds 3. The method according to claim 1, characterized in that the alkali metal compounds are introduced into the carbon black products when cooled with water. is introduced into the stream of carbon black products after its expansion at 800–1400 ° C, and before it is separated, into the carbon black gases when they are cooled 2. The method according to claim 1, characterized in that the total amount of metal compounds is 0.005-0.500% by weight of the raw material, 3. The method according to claim 1, characterized in that the alkali metal compounds are introduced into the carbon black products when cooled with water. 1The temperature of the pre-cooling of soot eaerah products, "C 2The temperature at which an additional amount of alkali metal compounds is introduced, ° C 3 Total amount of sodium hydroxide, X to the amount of raw material 4Number of sodium hydroxide (driven at the first stage, X from the general 5The amount of sodium hydroxide, added in addition, Z of total 6 Total amount of potassium hydroxide, X to quantities / raw 7 Total amount of potassium nitrate, X to the amount of raw materials 8 Total amount of potassium carbonate, X to the amount of raw materials 9 Total amount of sodium nitrate, X to the amount of raw material 10 Output of carbon black, X to raw materials Physical and chemical properties of carbon black according to GOST 7885- 36, GOST 25696.1-83, GOST-25699.14-83 11Roughness Specific surface, m / g: 12geometric 13 adsorption (for phenyl) 14vneshne 15 absorption (pa nitrogen) 16yodnoe, u / g 17Absorption di-Utilta 1100 1450 1400 1300 800 750 1100 1100 1100 1100 1100 1100 1100 600 600 600 600 600 600 180 200 350 550 750 780 600 600 0.025 0.01 0.05 0.1 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.004 0.005 686868686868686868686868686868 32323232323232323232323232 48.4 1.65 93 141 92 145,100 48.0 1.71 92 147 93 151 100 94 135 94 143 98 93 133 94 141 102 99 115 107 11,117 92 140 95 144 103 99 117 106 118,117 99 .116 108 113 software 99 116 107 142,117 93 139 96 142,100 93 140 91 143 107 100 114 lit 115 114 99 OF 117 114,115 100 112 software 113,116 98 114 109 115,116 92 138 93 136 109 136 93 137 103 48.7 49.1 54.2 52.0 54.0 54.8 54.1 48.0 48.6 53.2 53.8 54.1 53.9 48.8 52.3 53.0 1.60 1 , 58 1.49 1.36 1.19 1.15 1.15 1.52 1.53 1.15 1.15 1.13 1.16 1.48 1.46 1.07 1.44 1.07 115 112 107 119 1100 1450 1400 1300 800 750 1100 1100 1100 1100 1100 1100 1100 1100 vD 686868686868686868686868686868 32323232323232323232323232 Ov NJ U) VO about vO 48.0 1.71 48.7 49.1 54.2 52.0 54.0 54.8 54.1 48.0 48.6 53.2 53.8 54.1 53.9 48.8 52.3 53.0 1.60 1 , 58 1.49 1.36 1.19 1.15 1.15 1.52 1.53 1.15 1.15 1.13 1.16 1.48 1.46 1.07 92 147 93 151 100 94 135 94 143 98 93 133 94 141 102 99 115 107 11,117 92 140 95 144 103 99 117 106 118,117 99 .116 108 113 software 99 116 107 142,117 93 139 96 142,100 93 140 91 143 107 100 114 lit 115 114 99 OF 117 114,115 100 112 software 113,116 98 114 109 115,116 92 138 93 136 109 136 93 137 103 1.44 1.07 115 112 107 119 4 Amount of hydroxide aatrk, “driven on stage, Z of total 3. The amount of hydroxide hydrochloride. introduced additional yuggel about. Z oooojero 6Single amount of potassium hydro-yen, Z to the amount of raw material 7On its amount of nitrate pegs, Z to the amount of raw materials 8 Total amount of carbon potassium, Z to the amount of raw material 6868966896958050252068686S68 3232432452050758032323232 0.025 0.025 0.025 9 Total amount of sodium nitrate, Z to the amount of raw material 10 Soot output, raw materials Physicochemical properties of soot according to GOST 788 36, GOST 25696.1-83, GOST 25699.14-8J 11Roughness Specific surface, n / g: 12geometric 13 adsorption (for phenol) 14vneshne 15 absorbing (nitrogen) 16 Single number, mg / g 17 AA dibutyl phthalate adsorption, ml / 100 g carbon black 18 pH aqueous suspension 19 Ash content, Z 20 Voltage at 3001 nominal elongation, kgf / sy2 21Durability at break, kgf / cm 0.025 55, 55.2 53.7, | 7 1.16 1.17 1.17 1.16 1.17 54.2 51.0 52.0 53.0 54.0 56.0 56.0 53.0 53.0 52.6 64.0 1.16 1.74 1.08 1.08 1.05 1, 04 1.70 1.14 1.10 1.13 1.14 101 93 Y9 100 104 103 94 100 101 99 101 Uj o about vd Breathless About 1 L sh well AND sh sh EShSh Raw material Gaseous products Soto sh I H