CN1033930C - A method for evaluating ethylene feedstock - Google Patents
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- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 239000005977 Ethylene Substances 0.000 title claims abstract description 21
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Abstract
本发明公开了一种用微型脉冲裂解气相色谱技术评价乙烯原料的方法，它包括直接使用已知原料的工业炉各个产物收率数据与调整后的微型裂解条件下的已知原料脉冲裂解相应产物色谱峰面积之比作为求得未知原料各单项产物收率的校正因子，然后用等量的未知原料脉冲裂解后给出的色谱峰面积和校正因子计算产物收率，国际专利分类号为GO1N30/00。The invention discloses a method for evaluating ethylene raw materials by using micro-pulse cracking gas chromatography technology, which includes directly using the yield data of each product in an industrial furnace with known raw materials and the corresponding products of pulse cracking of known raw materials under adjusted micro-cracking conditions The ratio of the chromatographic peak area is used as the correction factor to obtain the yield of each single product of the unknown raw material, and then the product yield is calculated by using the chromatographic peak area and the correction factor given after the pulse cracking of the same amount of the unknown raw material. The international patent classification number is GO1N30/ 00.
Description
本发明涉及一种用微型脉冲裂解气相色谱技术评价乙烯原料的方法，特别是涉及一种用微量原料脉冲裂解的结果模拟大型工业裂解炉产物分布并预测被评价原料在工业裂解炉中主要产物收率的方法，适合于在脉冲式微型裂解——气相色谱系统上评价乙烯原料的实验过程。The present invention relates to a method for evaluating ethylene raw material by using micro-pulse cracking gas chromatography technology, in particular to a method for simulating the product distribution of a large-scale industrial cracking furnace and predicting the main product yield of the evaluated raw material in the industrial cracking furnace by using the pulse cracking result of a small amount of raw material. The rate method is suitable for the experimental process of evaluating ethylene feedstock on the pulsed micro-cracking-gas chromatography system.
众所周知，为了给大型工业裂解炉提供优质、合格的乙烯原料，保证足够高的乙烯和其他烯烃、芳烃收率，乙烯原料一般都需经过预先的评价和筛选。例如各种类型的模拟试验炉就是通过小型的连续式管式裂解炉来模拟大型工业裂解炉的裂解条件和裂解结果的。这些评价乙烯原料的过程一般都较复杂，费时、费工，花费也较昂贵，1978年Greco在色谱科学杂志(J.Chromatog.Sci.，16，(1978)，36)首先提出了一种用微型反应器与气相色谱仪连接的脉冲式微型裂解系统评价乙烯原料的方法，他仅用微量的石脑油乙烯原料脉冲在载气携带下进入微型裂解器中进行裂解，裂解产物直接进入气相色谱仪分析，经数据处理得到产物收率，他发现如此得到的乙烯收率与同一种原料在工业裂解炉上的乙烯收率存在线性关系。1979年Martens等人在烃加工杂志(HydrocarbonProcessing，58，(1979)，199)也报导了类似的乙烯原料评价方法但未涉及实验细节。1986年董鹏等人在第二次全国石油化工色谱学术报告会首先报导了(文集(1986)，423页)在改进了的微型裂解系统上经过精细地调整微型裂解参数可以同时使微量原料脉冲裂解后的几乎全部气体产物收率与工业裂解炉非常接近，因此提出了用微量原料脉冲裂解的结果直接模拟和预测工业炉产物收率的方法。此后邹仁鋆(化工机械，15卷，1988年6期)，高忠良等人(科学通报，1990年5期394页)也肯定和报导了类似的方法。用脉冲式微型裂解系统评价乙烯原料的方法快速、简便、花费低廉。这种方法的原则步骤是先选择一种已知工业裂解炉条件和主要产物收率的乙烯原料作为参照原料，调整微型裂解反应参数使参照原料脉冲裂解后的产物收率与在工业炉上的结果相近，然后在相同条件下裂解未知原料，即可预测出未知原料在同条件工业炉上的产物收率。要实现上述步骤的一个关键是如何把微量原料脉冲裂解后的产物检测信号转换成对原料的收率。过去一直延用的办法是配制一种已知某成分重量百分含量(即相当于对原料收率)的混合液态烃作外标样品，已知成分能单独给出色谱检测信号，在选择的裂解条件下用与原料等量的外标样脉冲进料先在低温下(避免标样裂解)求得单位色谱检测信号值(通常用峰面积积分数字)所相当的产物对原料收率，即校正因子，然后再把反应温度升高到适当程度进行原料脉冲裂解，把每个产物得到的色谱检测信号值分别乘以校正因子即得到这些产物对原料的收率。然而实践表明，尽管裂解一次原料脉冲的实验周期很短，但配制外标样和求取校正因子往往需要花费更多的时间，特别是要使原料脉冲裂解的产物收率与工业炉一致，经常需要反复调整微型裂解参数，反复进行裂解，而除了调整温度参数以外的任何参数调整，如脉冲量，停留时间，压力，色谱参数等，都可能改变校正因子测定的基准，因此校正因子往往需要在调整后的条件下降低反应器温度重新测定才能得到可靠的裂解产物收率。此外，除了检测信号的积分数字外，色谱积分仪用于日常分析的通用计算程序难以直接用到上述实验过程，还需要计算机对数据进行专门的处理。如此繁琐的操作步骤大大抵消了微型裂解技术的优越性，限制了它成为一种定型技术推广使用As we all know, in order to provide high-quality and qualified ethylene raw materials for large-scale industrial cracking furnaces and ensure a sufficiently high yield of ethylene, other olefins, and aromatics, ethylene raw materials generally need to be pre-evaluated and screened. For example, various types of simulated test furnaces simulate the cracking conditions and cracking results of large-scale industrial cracking furnaces through small continuous tubular cracking furnaces. These processes for evaluating ethylene raw materials are generally more complicated, time-consuming, labor-intensive, and expensive. In 1978, Greco first proposed a method for chromatographic science (J.Chromatog.Sci., 16, (1978), 36) The pulse type micro-cracking system connected with the micro-reactor and the gas chromatograph is a method for evaluating ethylene raw materials. It only uses a small amount of naphtha and ethylene raw material pulses to enter the micro-cracker under the carrier gas for cracking, and the cracked products directly enter the gas chromatograph. Instrument analysis, the product yield obtained through data processing, he found that there is a linear relationship between the ethylene yield obtained in this way and the ethylene yield of the same raw material on the industrial cracking furnace. In 1979, Martens et al. also reported a similar evaluation method for ethylene feedstock in the Journal of Hydrocarbon Processing (Hydrocarbon Processing, 58, (1979), 199), but did not involve experimental details. In 1986, Dong Peng and others first reported in the Second National Petrochemical Chromatography Academic Report (Collected Works (1986), page 423) that micro-cracking parameters can be finely adjusted on the improved micro-cracking system to simultaneously make trace raw materials pulse The yield of almost all gas products after cracking is very close to that of industrial cracking furnaces, so a method of directly simulating and predicting the product yields of industrial furnaces with the results of pulse cracking of trace raw materials is proposed. Afterwards Zou Renjun (Chemical Machinery, Volume 15, Issue 6, 1988), Gao Zhongliang et al. (Science Bulletin, Issue 5, 1990, page 394) also affirmed and reported a similar method. The method of evaluating ethylene feedstock with pulsed micro-cracking system is quick, simple and inexpensive. The principle step of this method is to select a kind of ethylene raw material with known industrial cracking furnace conditions and main product yield as the reference raw material, adjust the micro-cracking reaction parameters to make the product yield after pulse cracking of the reference raw material and the industrial furnace. The results are similar, and then the unknown raw material is cracked under the same conditions, and the product yield of the unknown raw material on the industrial furnace under the same conditions can be predicted. A key to realize the above steps is how to convert the detection signal of the product after the pulse cracking of the trace raw material into the yield of the raw material. The method that has been used in the past is to prepare a mixed liquid hydrocarbon with a known component weight percentage (that is, equivalent to the yield of the raw material) as an external standard sample. The known component can give a chromatographic detection signal alone. Under cracking conditions, use the same amount of external standard sample pulse feeding as the raw material to obtain the product to raw material yield equivalent to the unit chromatographic detection signal value (usually using the peak area integral number) at low temperature (to avoid standard sample cracking), namely Correction factor, then raise the reaction temperature to an appropriate level for raw material pulse cracking, and multiply the chromatographic detection signal value obtained by each product by the correction factor to obtain the yield of these products to the raw material. However, practice has shown that although the experimental period for cracking a raw material pulse is very short, it often takes more time to prepare external standard samples and obtain correction factors, especially to make the product yield of raw material pulse cracking consistent with industrial furnaces, often It is necessary to repeatedly adjust the micro-lysis parameters and repeat the cracking, and any parameter adjustment other than temperature parameters, such as pulse volume, residence time, pressure, chromatographic parameters, etc., may change the benchmark for the determination of the correction factor, so the correction factor often needs to be adjusted. Reliable cleavage product yields can only be obtained by lowering the reactor temperature and re-testing under the adjusted conditions. In addition, in addition to the integral number of detection signals, the general calculation program used by the chromatographic integrator for daily analysis is difficult to directly use the above-mentioned experimental process, and special processing of the data is required by the computer. Such cumbersome operation steps greatly offset the superiority of micro-cracking technology, limiting its popularization and use as a stereotyped technology
本发明的目的是提供一种用微型脉冲裂解气相色谱技术评价乙烯原料的方法，特别是一种改进的用微量原料脉冲裂解结果模拟工业裂解炉产物分布并预测乙烯原料在工业炉上产物收率的简捷方法，它不需要配制外标样，也不需要降低反应器温度来求取校正因子，并充分利用色谱积分仪的通用计算程序，因此大大简化了用微量原料脉冲裂解模拟工业裂解炉结果的步骤，节约了实验时间。The purpose of the present invention is to provide a method for evaluating ethylene raw materials with micro-pulse cracking gas chromatography technology, especially an improved method for simulating the product distribution of industrial cracking furnaces and predicting the product yield of ethylene raw materials on industrial furnaces by using the pulse cracking results of trace raw materials It does not need to prepare external standard samples, nor does it need to reduce the temperature of the reactor to obtain the correction factor, and makes full use of the general calculation program of the chromatographic integrator, so it greatly simplifies the results of simulating industrial cracking furnaces with pulse cracking of trace raw materials steps, saving experiment time.
本发明的目的是这样实现的：首先选择一种已知工业裂解条件下主要气体产物收率的乙烯原料作为参照原料，用这种参照原料在初步选择的微型裂解条件下裂解，各种产物的检测信号通过色谱积分仪立即给出一组以裂解气为主要成分的峰面积归一化数据，用这组数据与从相同成分工业裂解炉收率换算的归一化数据相对照即能判断微型裂解与工业炉裂解结果接近的程度，而无需取得各成分对原料的收率来加以比较。根据两种炉型归一化数据偏离程度进一步调整微型裂解反应参数，直到使裂解后的面积归一化数据与从工业炉计算的数据基本一致。实验证明，这时参照原料在微型裂解器上裂解产物对原料收率也会非常接近工业炉收率。利用色谱积分仪外标法的校正运转。将参照原料的工业炉数据输入积分仪即可得到对应成分的校正因子，即单位积分数字所代表的收率。然后在同一条件下用同一量的未知原料脉冲进行裂解，几分钟后色谱积分仪即可直接打印出与参照原料相同的工业裂解炉条件下未知原料各种产物的工业炉收率。The object of the present invention is achieved like this: at first select a kind of ethylene raw material of main gas product yield under the known industrial cracking condition as reference raw material, with this reference raw material cracking under the micro-cracking condition of primary selection, the yield of various products The detection signal immediately gives a set of normalized peak area data with cracked gas as the main component through the chromatographic integrator. By comparing this set of data with the normalized data converted from the yield of the industrial cracking furnace with the same component, the micro Cracking is close to the results of industrial furnace cracking, without the need to obtain the yield of each component to the raw material to compare. According to the degree of deviation of the normalized data of the two furnace types, the parameters of the micro-pyrolysis reaction were further adjusted until the normalized data of the area after pyrolysis was basically consistent with the data calculated from the industrial furnace. Experiments have proved that at this time, the yield of the pyrolysis product on the micro cracker with reference to the raw material will be very close to the yield of the industrial furnace. Calibration run using the external standard method of the chromatographic integrator. Input the industrial furnace data of the reference raw material into the integrator to obtain the correction factor of the corresponding component, that is, the yield represented by the unit integral number. Then use the same amount of unknown raw material pulse cracking under the same conditions, and after a few minutes, the chromatographic integrator can directly print out the industrial furnace yield of various products of the unknown raw material under the same industrial cracking furnace conditions as the reference raw material.
本发明与传统的原料脉冲裂解的外标定量的区别在于，本发明是利用裂解后气体产物的相对组成(峰面积归一化数据)来判断与工业炉结果接近程度的，因此无需在模拟工业炉过程中对参照原料脉冲裂解产物收率进行定量，而随后定量校正因子的求取又直接利用了参照原料的工业炉数据，因此省略了配制外标样和降温求取校正因子的麻烦，并且不需要专门的数据处理系统，大大节约了实验时间，易于在乙烯生产现场和科研中推广使用。上述这些区别也就是本发明的优点和效果。The difference between the present invention and the external standard quantity of the traditional raw material pulse cracking is that the present invention uses the relative composition (peak area normalized data) of the gas product after cracking to judge the closeness to the result of the industrial furnace, so there is no need to simulate the industrial furnace. During the furnace process, the yield of the pulse cracking product of the reference raw material is quantified, and the subsequent calculation of the quantitative correction factor directly uses the industrial furnace data of the reference raw material, so the trouble of preparing an external standard sample and lowering the temperature to obtain the correction factor is omitted, and It does not require a special data processing system, greatly saves experiment time, and is easy to be popularized and used in ethylene production sites and scientific research. The above-mentioned differences are the advantages and effects of the present invention.
下面的实施例是对本发明的进一步说明，而不是限制本发明。The following examples are to further illustrate the present invention, but not to limit the present invention.
实施例1：用已知原料脉冲裂解模拟工业裂解炉产物分布选择一种工业在用的轻柴油裂解原料R为已知参照原料，根据下表的已知工业裂解炉产物收率数据换算成裂解气相产物的相对组成，该组成成分与微型裂解能提供的色谱分析组成成分相对应。调整微型裂解参数使裂解后产物的色谱峰面积归一化数据与工业炉接近，其结果也列在表中。为验证模拟结果的可靠性，表中还列出了同时用传统配制液体外标定量法所给出的产物对原料的收率作为对照。
以上实验条件为：微型裂解炉管材质为2毫米内径石英管，微量原料脉冲量为0.4微升，原料汽化温度为350℃，反应载气为高纯氮，柱后载气流速60毫升/分，色谱柱填料为活性氧化铝，检测器为串联的热导和火焰离子化检测器，柱箱温度140℃，检测室温度200℃，外标样的成分为正戊烷，含量7％，传统校正因子测定温度为500℃。The above experimental conditions are: the material of the micro cracking furnace tube is 2 mm inner diameter quartz tube, the pulse volume of the trace raw material is 0.4 microliters, the vaporization temperature of the raw material is 350 ° C, the reaction carrier gas is high-purity nitrogen, and the carrier gas flow rate after the column is 60 ml/min , the chromatographic column filler is activated alumina, the detector is a thermal conductivity and flame ionization detector connected in series, the oven temperature is 140°C, the detection chamber temperature is 200°C, and the external standard sample is n-pentane with a content of 7%. The correction factor was measured at a temperature of 500°C.
实施例2-6：Embodiment 2-6:
将已知原料R的工业炉产物收率当作外标样已知成分含量数据输入色谱积分仪，在与例一完全相同的实验条件下重复裂解R原料三次，作为色谱积分仪的校正运转，其校正因子由积分仪自行求取和存贮。The industrial furnace product yield of the known raw material R is used as the known component content data of the external standard sample to input the chromatographic integrator, and the cracking R raw material is repeated three times under the same experimental conditions as Example 1, as the calibration operation of the chromatographic integrator, The correction factor is obtained and stored by the integrator itself.
选择了五种性质各异但与已知原料R馏分相当的轻柴油A、B、C、D作为未知原料，在已模拟了工业炉裂解结果的条件下分别用相同的微量脉冲量裂解这些原料，每种原料至少重复裂解了三次，积分仪按外标法模式处理数据，结果取平均值列入下表。为验证预测的可靠性，将五种原料用传统配制液体外标定量的方法所得数据和在连续式小型模拟试验炉的结果也对照列入表中。Five kinds of light oil oils A, B, C, and D, which have different properties but are equivalent to the known raw material R fraction, were selected as unknown raw materials, and these raw materials were cracked with the same micro-pulse amount under the conditions of simulating the cracking results of industrial furnaces. , each raw material was pyrolyzed at least three times, and the integrator processed the data according to the external standard method mode, and the results were averaged and listed in the table below. In order to verify the reliability of the prediction, the data obtained by the traditional method of preparing liquid external standard for the five raw materials and the results in the continuous small-scale simulation test furnace are also listed in the table.
表中全部数据均为裂解产物对原料收率(m％)。方法I为本发明方法，方法II为配制液体外标法，方法III为连续式小型模拟试验炉法。All the data in the table are cracked product to raw material yield (m%). Method I is the method of the present invention, method II is the method of preparing a liquid external standard, and method III is the continuous small-scale simulated test furnace method.
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|---|---|---|---|---|
| US8011238B2 (en) * | 2008-10-09 | 2011-09-06 | Chevron U.S.A. Inc. | Method for correcting the measured concentrations of gas components in drilling mud |
| CN101738447B (en) * | 2008-11-05 | 2013-05-01 | 重庆华邦制药有限公司 | Method for determining content of compound by utilizing relative correction factor |
-
1993
- 1993-10-22 CN CN 93118732 patent/CN1033930C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1086015A (en) | 1994-04-27 |
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